Knauer Azura RID 2.1L User manual

Detector RID 2.1L
User Manual
V6750

RID 2.1L user manual V6750, version 1.0
Table of Contents 3
Table of Contents
Note: For your own safety, read the manual and always observe the warnings and safety information on
the device and in the manual.
Product Information. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
Device Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
Features . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
Functional Principle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
Detector Design and Optical Path . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
Calculating the Signal Value . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
Flow Path . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
Intended Use . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
Eluents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
Safety for Users. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
Signal Words . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
Decontamination . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
Installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
Preparations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
Location Requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
Power Connection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
Scope of Delivery . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
Unpacking the Device . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
Connecting the Leak Management . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
Connecting the Capillaries . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
Integrating the Detector into a System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
Computer Control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
Configuring the LAN Settings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
Connecting the Cables . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
Configuring the Router . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
Integrating the LAN into a Company Network . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
Controlling Several Systems Separately in a LAN . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
Setting a static IP Address . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
Remote Control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
Connector Assignments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
Connecting the Cables to the Terminal Strip . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
Integrator Connector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
Meaning of the LEDs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
Default Settings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
Autozero . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
Temperature Control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
Signal Mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
Time Constant & Data Rate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
LED Power Factor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
Extended Dynamic Range . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
Analog Output Scaling and Offset . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26

RID 2.1L user manual V6750, version 1.0
4TableofContents
GLP . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
Starting the Detector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
Flushing the Flow Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
Activating the Standby . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
Stopping the Detector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
Functional Tests . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
Diagnostics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
LAN . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30
Device Problems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30
System Messages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
Proceeding with Tasks after a Leak . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32
Maintenance. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32
User Tasks and Intervals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33
Checking the Calibration/Validation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33
Preparing for Storage or Transport . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
Legal Information. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
Transport Damage . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
Warranty Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
Declaration of Conformity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
Warranty Seal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
Disposal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
Technical Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36
Repeat Orders. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
HPLC Glossary. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38
Index . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40

RID 2.1L user manual V6750, version 1.0
Product Information 5
Product Information
The AZURA RID 2.1L is a sensitive and competitively priced differential
refractometer suitable for detecting compounds with litte or no UV activity
such as alcohols, sugars, lipids or polymers.
AZURA L features The RID 2.1L is a member in the AZURA L product line and shares a number
of common features:
Removable front cover, for optional device and/or operator protection;
Instrument stability through a large base area and low center of gravity;
Intelligent leak management consisting of a leak sensor and safe leak
handling;
LED device status indication;
Power connection and control connectors on rear of device.
Identification The device name RID 2.1L can be found on the front panel, above the serial
number. A silver sticker on the rear side displays the manufacturer name and
address, the product number and power supply specifications.
Safety symbols Pay particular attention to the warnings that are highlighted in the figures
below. The leak tray can carry a maximum of 500 g/0.5 kg. If any errors
require the opening of the housing, the device must be turned off in
advance. Use the main switch on the rear to turn the device on/off.
Note: Only trained service technicians are permitted to open the housing
and carry out maintenance on the interior components of the device.
Device Overview
Legend
1OUT port
2IN port
3LED panel with standby
key (see page 22)
4Leak tray
5Capillary guides
Fig. 1 front view
23
4
5
1

RID 2.1L user manual V6750, version 1.0
6 Product Information
Features
Optical bench The newly designed optical unit with advanced temperature control ensures
high sensitivity, fast baseline stabilization, and excellent reproducibility. Fur-
thermore, the long-life LED, and highly back pressure resistant flow cell
guarantee minimal maintenance.
Extended dynamic range Upon activating the extended dynamic range option, it is possible to
broaden the linear dynamic range.
Data rate The detector measures with a maximum data rate of 100 Hz. During the
measurement, 100 spectra per second are recorded.
Control This detector can be controlled with various Chromatography Data Systems
(OpenLAB® EZChrom Edition, ClarityChrom®, Chromeleon®, Purity-
Chrom® Bio and Mobile Control Chrom), as well as from an optional touch
display (Mobile Control), via LAN or through analog input/output, allowing
it to be integrated into almost any LC system.
GLP data The Mobile Control and supported software products can be used to display
or read out GLP data such as operating hours, light source operating hours,
etc. You can find a detailed description on how to display or read out GLP
data from your device in the respective user manuals.
Diagnostics Light intensity and balance, zero glass position and LED current can be eas-
ily monitored via the Mobile Control and supported software products to
ensure optimal working conditions for your analysis.
Legend
1Integrator output
2Service interface (USB)
3LAN and switch con-
nector 1
4LAN and switch con-
nector 2
5Multi-pin connector
6Connection and main
switch
Fig. 2 rear view
7Rear label
12 34
56
7

RID 2.1L user manual V6750, version 1.0
Product Information 7
AZURA Neo The AZURA Neo electronic platform features:
A new microprocessor for faster device performance
New interfaces: dual IP stack with switch (for connecting AZURA devices
to one another) and LAN stack function, plus USB (internal USB to RS-
232) service interface.
Industrial standard 4–20 mA analog input (replacing 0–10 V input on the
previous electronic platform).
No external display support.
Functional Principle
When a ray of light passes from one medium into another the light is
refracted or bent depending on the light ray’s speed of light and the angle
of incidence. The extent to which a medium refracts light is its refractive
index (RI). Snell’s law of refraction expresses the relationship between the
angle of incidence and the angle of refraction.
Snell’s Law of refraction
where
α
1angle of incidence
α
2angle of refraction
c1speed of light in medium 1
c2speed of light in medium 2
n1refractive index in medium 1
n2refractive index in medium 2
nrelative refractive index
The refractive index of a medium depends on the wavelength of the light
and the density of the medium. Normally, in an RI detector, the wavelength
is constant. The density depends on the temperature, pressure and compo-
sition of the medium.
Detector Design and Optical Path
The AZURA RID 2.1L is a differencial refractive index detector of the deflec-
tion type. The detector measures the deflection of a light beam causes by
the difference in refractive index between the liquids in sample and refer-
ence cell compartments of the flow cell.
A light beam emitted from the LED light source 1crosses the RID’s sample
and the reference cells 2twice. When both cells contain pure solvent, the
system is calibrated to zero by means of a parallel zero glass plate 3which
positions the beam on the two detector diodes 4in such a manner that the
measured light intensities (I1and I2) of the two diodes are virtually identical.
α
1
sin
α
2
sin
-------------- c1
c2
-----n1
n2
------n== =

RID 2.1L user manual V6750, version 1.0
8 Product Information
When the sample cell contains a solution with a different refractive index,
the light beam is geometrically proportionally deflected depending on the
relative change of the refractive index (according to Snell´s law).
This results in a change of the light intensities I1and I2(one increases and
the other decreases), proportional to concentration and refractive index of
the sample solution. From these intensity changes the signal value is calcu-
lated.
Calculating the Signal Value
The light beam reaches the two detector diodes (1 and 2) which deliver the
intensity values I1and I2during measurement, depending on the light
beam’s deflection. The difference and sum of I1and I2are calculated contin-
uously, and the resulting signal is given out to the device’s outputs.
Flow Path
Analysis During analysis the solvent takes the blue flow path (see figure below):
1. Enters through IN port.
2. Passes through heat exchanger.
3. Flows through sample compartment of the flow cell.
4. Passes through flush valve.
5. Exits through OUT port.
Flush active When the flush valve is activated the solvent takes the green flow path (see
figure below):
1. Enters through IN port.
2. Passes through heat exchanger.
3. Flows through sample compartment of the flow cell.
4. Passes through flush valve and directed to the second heat exchanger.
5. Flows through reference compartment of the flow cell.
6. Exits through OUT port.
Signal Value
I1–I2difference of intensity values
I1+I2sum of intensity values
aautozero constant
ccalibration constant
1
2
3
4
signal I1I–2
()
I1I2
+()
-------------------- a+



c×=

RID 2.1L user manual V6750, version 1.0
Product Information 9
Intended Use
Refractive index (RI) detection is best suited for use in analytical HPLC (high
performance liquid chromatography), GPC (gel permeation chromatogra-
phy) as well as SEC (size-exclusion chromatography) applications.
RI detectors deliver a universal response, however detection is intrinsically
less sensitive than other detection methods. RI detectors are not suited for
gradient chromatography as they are very sensitive to changes in the eluent
composition. Furthermore, RI detectors are highly temperature and pressure
dependent, and unstable conditions can lead to baseline instability. It is also
possible that positive and negative peaks appear in a single analysis.
The device is designed for research purposes and may not be suitable for
diagnostic analysis.
Operating range Note: Only use the device for applications that fall within the range of the
intended use. Otherwise, the protective and safety equipment of the device
could fail.
The detector can be used for analytical applications (with flow rates up to
10 ml/min) in the following areas:
food analysis
chemical analysis
pharmaceutical analysis
environmental analysis
biochemical analysis
Eluents
Even though the AZURA RID 2.1L is very resistant to many kinds of com-
monly used eluents, you should take care that no eluent or water can get on
the device’s surface or even inside the device. Chlorinated hydrocarbons
could destroy the varnish and some others (e. g. THF) could loosen certain
components. Even small quantities of other substances, such as additives,
modifiers, or salts can influence the durability of the materials.
Usage of well degassed eluents is very important for achieving good chro-
matograms with an RI detector. Degassing ensures a stable baseline and
high sensitivity.
Note: The user is responsible for the adequate and safe use of any liquids
and chemicals. The solvent list contains the solvents KNAUER recommends
Legend
1solvent
2heat exchanger
3sample cell
4reference cell
5flush valve
6waste
7temperature con-
trolled compartment
12
3
7
45
6

RID 2.1L user manual V6750, version 1.0
10 Safety for Users
for use. If there is any doubt, contact the Technical Support of the manufac-
turer.
Suitable solvents This is the list of eluents you can use without any concern:
acetate buffer solutions
acetone at 4 °C-25 °C (39.2 °C-77.0 °F)1
acetonitrile2
benzene
chloroform
ethyl acetate
ethanol
formiate buffer solution
isopropanol
carbon dioxide (liquid 99.999 % CO2)
methanol
phosphate buffer solutions (0.5 M)
toluol
ammoniated dilute solution
acetic acid (0.1-1 %), at 25 °C
sodium hydroxide (1 M)
water
Less suitable solvents This is the list of eluents you should rather not use:
diethylamine (0.1 %) (DEA)
dimethyl sulfoxide (DMSO)
methylene chloride3
phosphoric dilute acid
slightly volatile eluents
tetrahydrofuran (THF)3
triethylamine (0.1 %) (TEA)
trifluoroacetic acid (0.1 %) (TFA)
Not suitable solvents This is the list of eluents you should definitely not use:
concentrated mineral and organic acids
concentrated bases
eluents containing particles
halogenated hydrocarbons, e.g. Freon®
perfluorinated eluents, e.g. Fluorinert® FC-75, FC-40
perfluorinated polyether, e.g. Fomblin®
Safety for Users
Professional Group The user manual addresses persons who are qualified as chemical laboratory
technicians or have completed comparable vocational training.
The following knowledge is required:
Fundamental knowledge of liquid chromatography
Knowledge regarding substances that are suitable only to a limited
extent for use in liquid chromatography
Knowledge regarding the health risks of chemicals
Participation during an installation of a device or a training by the com-
pany KNAUER or an authorized company.
1. valid for the specified temperature range
2. not recommended in combination with PEEK small parts and PEEK capillaries
3. not recommended in combination with PEEK small parts and PEEK capillaries

RID 2.1L user manual V6750, version 1.0
Safety for Users 11
If you do not belong to this or a comparable professional group, you may
not perform the work described in this user manual under any circum-
stances. In this case, please contact your superior.
Safety Equipment When working with the device, take measures according to lab regulations
and wear protective clothing:
Safety glasses with side protection
Protective gloves
Lab coat
What must be taken into
account?
All safety instructions in the user manual
The environmental, installation, and connection specifications in the user
manual
National and international regulations pertaining to laboratory work
Original spare parts, tools, and solvents made or recommended by
KNAUER
Good Laboratory Practice (GLP)
Accident prevention regulations published by the accident insurance
companies for laboratory work
Filtration of substances under analysis
Use of inline filters
Once they have been used, never re-use capillaries in other areas of the
HPLC system.
Only use a given PEEK fitting for one specific port and never re-use it for
other ports. Always install new PEEK fittings on each separate port.
Follow KNAUER or manufacturer's instructions on caring for the columns
More safety-relevant information is listed below:
flammability: Organic solvents are highly flammable. Since capillaries can
detach from their screw fittings and allow solvent to escape, it is prohib-
ited to have any open flames near the analytical system.
solvent tray: Risk of electrical shock or short circuit if liquids get into the
device's interior. For this reason, place all bottles in a solvent tray.
solvent lines: Install capillaries and tubing in such a way that liquids can-
not get into the interior in case of a leak.
leaks: Regularly check if any system components are leaking.
power cable: Defective power cables are not to be used to connect the
device and the power supply system.
self-ignition point: Only use eluents that have a self-ignition point higher
than 150 °C under normal ambient conditions.
power strip: If several devices are connected to one power strip, always
consider the maximum power consumption of each device.
power supply: Only connect devices to voltage sources, whose voltage
equals the device's voltage.
toxicity: Organic eluents are toxic above a certain concentration. Ensure
that work areas are always well-ventilated! Wear protective gloves and
safety glasses when working on the device!
Where is use of the device
prohibited?
Never use the system in potentially explosive atmospheres without appro-
priate protective equipment. For further information, contact the Technical
Support of KNAUER.
Secure decommissioning At any time, take the device completely out of operation by either switching
off the power switch or by pulling the power plug.
Opening the Device The device may be opened by the KNAUER Technical Support or any com-
pany authorized by KNAUER only.