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Xdlib016en K Refguide Dma M v2.98 Web

This document provides instructions for operating DMA 4100/4500/5000 M density meters. It discusses safety, components, installation, operation, measurements, and maintenance. Key points include measuring liquids via the oscillating U-tube principle, defining measurement methods, performing checks and adjustments to ensure accuracy, and tips for taking high-precision density readings. The document aims to guide users in properly setting up and using the instruments.

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Noura
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© © All Rights Reserved
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Download as PDF, TXT or read online on Scribd
0% found this document useful (0 votes)
27 views68 pages

Xdlib016en K Refguide Dma M v2.98 Web

This document provides instructions for operating DMA 4100/4500/5000 M density meters. It discusses safety, components, installation, operation, measurements, and maintenance. Key points include measuring liquids via the oscillating U-tube principle, defining measurement methods, performing checks and adjustments to ensure accuracy, and tips for taking high-precision density readings. The document aims to guide users in properly setting up and using the instruments.

Uploaded by

Noura
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
You are on page 1/ 68

Measure

what is measurable
and make measurable
that which is not.
Galileo Galilei (1564-1642)

Reference Guide

DMA 4100 M
DMA 4500 M
DMA 5000 M
instrument software version: from 2.98
(Original Instructions)
Disclaimer
This document may contain errors and omissions. If you discover any such errors, or if you would like to see
more information in this document, please contact us at our address below. Anton Paar assumes no liability
for any errors or omissions in this document.

Changes, copyright, trademarks, etc.


This document and its contents may be changed or amended by Anton Paar at any time without prior notice.
All rights reserved (including translation). This document, or any part of it, may not be reproduced, changed,
copied, or distributed by means of electronic systems in any form (print, photocopy, microfilm, or any other
process) without prior written permission by Anton Paar GmbH.
Trademarks, registered trademarks, trade names, etc. may be used in this document without being marked
as such. They are the property of their respective owner.

Further information
Published and printed by Anton Paar GmbH, Austria
Copyright © 2022 Anton Paar GmbH, Graz, Austria
Address of the instrument producer: Anton Paar GmbH
Anton-Paar-Str. 20
A-8054 Graz / Austria – Europe
Tel: +43 (0) 316 257-0
Fax: +43 (0) 316 257-257
E-Mail: info@anton-paar.com
Web: www.anton-paar.com

Date: July 14, 2022


Document number: XDLIB016EN-K
Contents

Contents
1 Safety Instructions ................................................................................................................................ 5
2 DMA 4100/4500/5000 M – An Overview ............................................................................................... 7
2.1 Measuring Principle ........................................................................................................................ 8
2.2 Functional Components .................................................................................................................. 9
3 Checking the Supplied Parts ............................................................................................................. 11
4 Installing the Instrument .................................................................................................................... 14
4.1 Installation Requirements ............................................................................................................. 14
4.2 Mounting the Injection Adapters ................................................................................................... 14
4.3 Leak Tightness Test ...................................................................................................................... 15
4.4 Mounting the Hoses ...................................................................................................................... 15
4.5 Connecting the Cooling ................................................................................................................. 16
4.6 Power Connection ......................................................................................................................... 16
4.7 Switching the Instrument On/Off ................................................................................................... 16
4.8 Basic Instrument Settings / First Checks ...................................................................................... 17
5 Operating the Instrument ................................................................................................................... 18
5.1 Operating Elements on the Main Screen ...................................................................................... 18
5.2 Operating Elements on the Menu Screen ..................................................................................... 20
6 Camera Settings .................................................................................................................................. 21
6.1 Adjusting the Camera Position ...................................................................................................... 21
6.2 Setting the Camera Illumination .................................................................................................... 21
6.3 Saving a Camera Picture .............................................................................................................. 21
7 Defining and Using Methods ............................................................................................................. 22
7.1 Measuring Methods ...................................................................................................................... 22
7.2 Changing Methods ........................................................................................................................ 23
7.2.1 Measurement Settings of the Density Module ...................................................................... 23
7.2.2 Defining Measurement Settings ............................................................................................ 24
7.2.3 Defining the Measurement Mode .......................................................................................... 24
7.2.4 Defining Formula Parameters ............................................................................................... 27
8 Performing a Measurement ................................................................................................................ 28
8.1 Sample Name ............................................................................................................................... 28
8.2 Filling Samples .............................................................................................................................. 28
8.3 Measurement Procedure .............................................................................................................. 30
8.4 Filling and Measurement Warnings .............................................................................................. 30
8.4.1 Status Messages .................................................................................................................. 30
8.4.2 Warning Messages ............................................................................................................... 31
8.5 Tips for Highly Accurate Density Measurements .......................................................................... 31
8.6 Degassing Samples ...................................................................................................................... 33
8.7 Special Filling Techniques ............................................................................................................ 33
8.8 Measuring at Low Temperatures / under High Humidity Conditions ............................................. 34
8.8.1 Preventing Condensation in the Measuring Cell ................................................................... 34
8.8.2 Removing Condensation From the Camera ......................................................................... 34
8.8.3 Preventing Condensation in the Measuring Cell Block ......................................................... 35
8.9 Measuring at High Temperatures ................................................................................................. 35
8.10 Measuring at High Pressures ...................................................................................................... 35
9 Checks, Adjustments, Calibrations ................................................................................................... 36
9.1 Definitions ..................................................................................................................................... 36
9.2 Checks .......................................................................................................................................... 36
9.2.1 Check Settings ...................................................................................................................... 36
9.2.2 Performing a Check .............................................................................................................. 37
9.2.3 Auto Air Check ...................................................................................................................... 38
9.2.4 Viewing, Printing, or Exporting Current Check Data ............................................................. 38

XDLIB016EN-K 3
Contents

9.3 Adjustments .................................................................................................................................. 39


9.3.1 Air/Water Adjustment ............................................................................................................ 39
9.3.2 Air/Water Wide-Range Adjustment ....................................................................................... 40
9.3.3 Adjustment of the Built-in Atmospheric Pressure Sensor ..................................................... 40
9.3.4 Performing Special Adjustments ........................................................................................... 40
9.3.4.1 Special Adjustments ..................................................................................................... 40
9.3.4.2 Special Adjustment for the Canadian Excise Alcohol Table ......................................... 41
9.3.5 Viewing, Printing, or Exporting Adjustment Data .................................................................. 42
9.3.6 Viewing, Printing, or Exporting Adjustment History: Adjustment Trend ................................ 42
9.3.7 Resetting the Adjustment Data to Factory Adjustment ......................................................... 42
9.3.8 Adjustment Analysis .............................................................................................................. 42
9.4 Calibration ..................................................................................................................................... 43
10 Upkeep and Cleaning ........................................................................................................................ 44
10.1 Cleaning and Drying the Measuring Cell .................................................................................... 44
10.2 Cleaning the Instrument Housing and the Touchscreen ............................................................. 45
10.3 Storing the Instrument ................................................................................................................. 45
10.4 Transporting the Instrument ........................................................................................................ 45
11 Maintenance and Repair ................................................................................................................... 46
11.1 Maintenance Performed by an Authorized Anton Paar Service Engineer .................................. 46
11.2 Repair Performed by an Authorized Anton Paar Representative ............................................... 46
Appendix A: Technical Data .................................................................................................................. 47
A.1: Specifications .............................................................................................................................. 47
A.2: Instrument Data and Operating Conditions ................................................................................. 48
A.3: Wetted Parts ................................................................................................................................ 49
Appendix B: Output Quantities and Live Raw Data ............................................................................ 50
B.1: Output Quantities ......................................................................................................................... 50
B.2: Live Raw Data ............................................................................................................................. 54
Appendix C: List of Quick Settings Parameters ................................................................................. 55
Appendix D: Density Tables .................................................................................................................. 57
D.1: Density of Air ............................................................................................................................... 57
D.2: Density of Water (0 °C to 100 °C) ............................................................................................... 58
Appendix E: List of Typical Samples and Recommended Cleaning Liquids ................................... 60
Appendix F: Troubleshooting ............................................................................................................... 62
Appendix G: Menu Tree ......................................................................................................................... 65
Appendix H: EU Declaration of Conformity ......................................................................................... 68

4 XDLIB016EN-K
1 Safety Instructions

See the General Software Functions Manual for a comprehensive description of the instrument software and
instructions for its use.
Download Anton Paar documents for free from the Anton Paar website: https://www.anton-paar.com

1 Safety Instructions
• Read the documentation before using the instru- • Use only accessories, consumables, or spare
ment.. parts supplied or approved by Anton Paar
• Follow all hints and instructions in the docu- GmbH.
mentation to ensure the correct use and safe • Ensure that all operators have been trained
functioning of the instrument. beforehand to use the instrument safely and
• The documentation is a part of the product. correctly.
Keep it for the complete working life of the prod- • Ensure that the instrument is sufficiently super-
uct and make it easily accessible for all persons vised during operation.
involved with the product. If you receive any • In case of damage or malfunction, do not con-
additions or revisions to the documentation from tinue operating the instrument. Do not operate
Anton Paar GmbH, these must be treated as the instrument under conditions which could
part of the documentation. result in damage to goods or injuries or loss of
life.
1.1 Liability • If liquid has been spilled over the instrument,
disconnect the instrument from the AC power
• This document does not claim to address all supply. Clean and dry the housing of the instru-
safety issues associated with the use of the ment. If you have a suspicion that liquid got into
instrument and samples. It is your responsibility the instrument, have the instrument cleaned
to establish health and safety practices and to and checked for electrical safety by a service
determine the applicability of regulatory limita- technician authorized by Anton Paar GmbH.
tions.
• Anton Paar GmbH only warrants the proper Operation in areas with risk of explosion
functioning of the instrument if no modifications • The instrument is not explosion-proof and
are made to mechanics, electronics, or soft- therefore must not be operated in areas with
ware. risk of explosion.
• Use the instrument only for the purpose de-
scribed in the documentation. Anton Paar GmbH Operation with explosive samples
is not liable for damages caused by incorrect use
of the instrument. • The instrument must not be used for the mea-
surement of samples of explosion group IIC
• The results delivered by the instrument depend
(such as carbon disulfide or acetylene).
not only on the correct functioning of the instru-
ment, but also on various other factors. We
therefore recommend that you have the results General precautions
checked (e.g. plausibility tested) by skilled
• Observe and adhere to your national safety
persons before consequential actions are taken
regulations regarding the handling of all sub-
based on the results.
stances associated with your measurements
(e.g. use safety goggles, gloves, respiratory
protection, etc.).
1.2 Installation and Use
• Before a measurement check the wetted parts
• The installation procedure shall be carried out of the instrument for chemical resistance to the
only by authorized persons who are familiar samples and cleaning agents used.
with the installation instructions.

XDLIB016EN-K 5
1 Safety Instructions

• Take care that the liquids (samples and cleaning • To move or lift the instrument, grasp the ledge
agents) or gases that you use are chemically on top of the instrument at the back with one
compatible when they come into contact with hand. Place the other hand under the display at
each other. They must not react exothermally or the front. There is a hollow for your fingers.
produce solid particles, which might stick to the • Carry the instrument in front of you and keep it
inner walls of the measuring cells. close to your body.
• Before you start a measurement or cleaning
procedure, take care that all parts, in particular
the measuring cells, the injection adapters, the 1.3 Service and Repairs
hoses, and the waste vessel, are properly con-
nected and in good condition. • Service and repair procedures may be carried
• Before you start a measurement or cleaning out only by authorized persons or by Anton Paar
procedure, check the injection adapters for leak GmbH.
tightness.
• Take measures that spilled liquids cannot get 1.4 Disposal
into plug connections or venting slots of electri-
cal appliances. • Concerning the disposal of the instrument,
• Connect the measuring system to the AC power observe the legal requirements in your country.
supply via a safety switch located at a safe dis-
tance from the instruments. In an emergency,
turn off the power using this switch instead of 1.5 Conventions for Safety Messages
the power switch on the instruments.
The following conventions for safety messages are
Precautions for flammable samples and used in this document:
cleaning agents
• Keep potential sources of ignition, like sparks or
open flames, at a safe distance from the instru-
WARNING
ment. Description of risk
• Place the instrument on a laboratory bench Warning indicates a hazardous situation which, if
made of fireproof material, preferably bricks, not avoided, could result in death or serious
ceramics, or stoneware. injury.
• Store only the minimum required amount of
sample, cleaning agents, and other flammable
materials near the instrument.
• Do not spill sample/cleaning agents or leave CAUTION
their containers uncovered. Immediately Description of risk
remove spilled sample/cleaning agents. Caution indicates a hazardous situation which, if
• Ensure that the setup location is sufficiently not avoided, could result in minor or moderate
ventilated. The environment of the instrument injury.
must be kept free from flammable gases and
vapors.
• Provide fire-extinguishing equipment. NOTICE
Description of risk
Notice indicates a situation which, if not avoided,
Transportation
could result in damage to property.
• Empty the measuring cell and all hoses before
you move or lift the instrument.

6 XDLIB016EN-K
2 DMA 4100/4500/5000 M – An Overview

2 DMA 4100/4500/5000 M – An Overview


The density measurement is based on the oscillat- • U-View™: Real-time images by a camera with
ing U-tube method, which has been first introduced zoom function enable you to visually inspect the
on the market by Anton Paar in 1967. measuring cell.
State-of-the-art digital density and concentration • The patented “Pulsed Excitation Method”
meters have been developed to combine highest (AT 516420 (B1)) even improves operational
precision with easy operation and robust design. safety, as the condition of the measuring cell
can be monitored in detail.
Your DMA M series instrument is equipped with the
world's most advanced digital density measurement
technology. This “Pulsed Excitation Method” and User interface
various features supporting your density measure- The touchscreen user interface facilitates easy and
ments are described below. intuitive operation in routine applications as well as
in demanding scientific research work:
Inside DMA 4100/4500/5000 M • For the most common applications, 10 measur-
• The oscillation periods of the U-tube and the ing methods are predefined. Just select the
reference oscillator are measured by optical method suiting your application, or create your
pickups. own methods.
• Two integrated Pt 100 platinum thermometers • Density values are automatically converted into
together with Peltier elements provide an concentration values for a large number of
extremely precise thermostatting of the sample. factory-programmed substances. You can add
further substances as required by yourself.
• ThermoBalance™: The additional reference
oscillator provides long-term stability and • Optionally operate DMA 4100/4500/5000 M via
enables precise measurements over the whole external keyboard, mouse, gesture control or
temperature range of the instrument, with only barcode reader.
one adjustment at 20 °C. • Optionally connect an external monitor or touch-
• Viscosity-related errors are automatically cor- screen (VGA interface).
rected over the full viscosity range by measuring Your DMA M series instrument can be converted
the damping effect caused by the viscous prop- into a measuring instrument completely and
erty of a sample. The result is subsequently permanently controlled by the PC software M Series
used for the calculation of the viscosity corrected Desktop. Contact your Anton Paar representative
density value. for detailed information.

Condition monitoring Compact and robust design


• The built-in sensor for the atmospheric pressure The instruments of the DMA M series are ready for
enables the automatic calculation of the current reliable measurements also in demanding environ-
air density required for adjustments and checks ments thanks to the following strengths:
of the instrument, as the air density is dependent
on the atmospheric pressure. • Compact design
• FillingCheck™: A major source of measuring • Sealed housing that withstands shocks, dirt,
errors with density meters are gas bubbles in the and spillages
measuring cell. The instrument automatically • Robust housing materials: coated aluminum
detects inhomogeneities and gas bubbles in the (top and sides), aluminum (base and back), and
whole measuring cell by an advanced analysis polystyrene/butadiene (front)
of its oscillation pattern. Where necessary, a
warning message is generated in real time for
every single measurement.

XDLIB016EN-K 7
2 DMA 4100/4500/5000 M – An Overview

2.1 Measuring Principle to any other oscillating U-tube method. The Pulsed
Excitation Method provides a viscosity correction
two times better than any other measuring principle,
Definition of density and specific gravity a better repeatability of the density result, and
detection of gas bubbles or particles in the sample.
The density ρ of a sample is defined as mass
divided by volume: Through precise and continuous monitoring of the
oscillation pattern during excitation and fade-out,
m followed by a mathematical conversion, the density
 = -----
V of the filled sample can be determined.
The specific gravity SG is calculated by dividing the The density ρ is calculated from the quotient of
density of a sample by the density of pure water at oscillation periods of the U-tube and the reference
a defined temperature: oscillator.

 sample 2
 = A  PQ  f 1 – B  f 2
SG = ------------------
 water
A, B .. instrument specific constants
Density and specific gravity are highly temperature- PQ.... oscillation period of the U-tube divided by the
dependent. oscillation period of the reference oscillator
f1, f2.. correction factors for temperature, viscosity
and nonlinearity
The oscillating U-tube method of
DMA 4100/4500/5000 M
Concentration measurement
stable oscillation In binary mixtures, the density of the mixture is a
function of its composition. Thus, the density value
of a binary mixture can be used to calculate its com-
position with the aid of density/concentration tables.
Amplitude

This is also possible with so-called quasi-binary mix-


tures. These are mixtures containing two major
components and some additional components pres-
ent in very small concentrations compared to the two
fade-out main components. Many decarbonated soft drinks,
excitation for example, can be considered to be quasi-binary
solutions of sugar in water, because the concentra-
Fig. 1: Outline of the Pulsed Excitation Method tion of flavors and acids are very small compared to
The sample is introduced into a U-shaped tube sugar and water. Hence the sugar concentration can
made of borosilicate glass that is being excited to be measured with a density meter.
oscillate at its characteristic frequency, which Note that the accuracy of the concentration mea-
changes with temperature and density of the filled surement depends not only on the accuracy of the
sample. After having reached a stable oscillation, instrument, but also on the slope of the density /
the excitation is switched off, and the oscillation concentration correlation. This means, for example,
fades out. The excitation and fade-out sequence is that a density measurement with an accuracy of
repeated continuously. This patented Pulsed Exci- ±0.00001 g/cm3 will be converted into an ethanol
tation Method (AT 516420 (B1)) allows the instru- value with a significantly smaller accuracy of
ment to determine the quality factor of the oscillating ±0.025 % w/w. The accuracy of some typical con-
U-tube in a sophisticated way that provides deeper centration measurements is given in appendix A.1.
insights into the sample’s characteristics compared

8 XDLIB016EN-K
2 DMA 4100/4500/5000 M – An Overview

2.2 Functional Components


Front and right side

2 3

1 5

Recessed grip for transportation

Fig. 2: View of the front and right side of DMA 5000 M

1 Power-on LED 4 Xsample slot cover plate


2 Color PCAP touchscreen 5 Sample inlet and outlet
3 Syringe holder (DMA 5000 M only) 6 Air pump outlet

Left side

1 2 3 1 2

Fig. 3: Views of the left side of DMA M | DMA M CK

1 Blind covers | Inlet and outlet connectors for the cooling kit
2 USB 2.0 sockets (type A), 3x
3 Protection cover for the USB sockets

XDLIB016EN-K 9
2 DMA 4100/4500/5000 M – An Overview

Rear

Ledge handle for transportation 1 2

4
5

14 6

13 12 11 10 9 8

Fig. 4: View of the rear of DMA 5000 M

1 “DRY AIR BLOCK” connectors 8 Power on/off switch


2 USB 2.0 socket (type A) 9 Fuse holder
3 VGA connector (DE-15F connector) 10 AC power jack
4 COM / RS-232 serial port (DE-9F connector) 11 UL test mark
5 Ethernet terminal (RJ45 connector) 12 Type plate with serial number
6 CAN interface (for the connection of further 13 Product number (P/N = mat. no.)
measuring modules) 14 Fan
7 “DRY AIR IN AIR PUMP” connector

10 XDLIB016EN-K
3 Checking the Supplied Parts

3 Checking the Supplied Parts


The instrument has been tested and packed care- 1. Keep the packaging material (box, foam pieces,
fully before shipment. However, damage may occur transport protection) for possible returns or for
during transportation. questions from the transportation or the insur-
ance company.
2. To check the delivery for completeness, com-
pare the supplied parts to those listed in table 1.
3. If a part is missing, contact your Anton Paar
representative.
4. If a part is damaged, contact the transportation
company and your Anton Paar representative.

Table 1: Supplied parts

Qty. Article description Mat. no.


1 DMA 4100 M 163378
or DMA 4500 M 176803
or DMA 5000 M 183345

or DMA 4100 M CK 176251


or DMA 4500 M CK 176804
or DMA 5000 M CK 185099
1 Power cable
1 Instruction Manual and Safety Information English 80812

1 Density standard ultra-pure water 5x10 mL 96044


with certificate

1 Waste vessel 500 mL 6210

XDLIB016EN-K 11
3 Checking the Supplied Parts

Table 1: Supplied parts (cont.)

Qty. Article description Mat. no.


1 Accessory kit DMA / DMA 4100/4500 M 159958
or
Accessory kit DMA 5000 M 186784

containing:
2m Hose 4x6 mm silicone (transparent) 57024
only for pressures up to 0.4 bar rel.

1 Hose 300x3x2 PTFE “AA” 3443


(only in accessory kit DMA 5000 M)

1 Hose 140x3x2 PTFE 2x¼"–28 UNF 187223


(only in accessory kit DMA 5000 M)
7 Syringe 2 mL Luer 51974

2 Injection adapter Luer black 159026


(in accessory kit DMA 4100/4500 M)

or
Injection adapter UNF ¼" black 159025
(in accessory kit DMA 5000 M)

2 Male Luer plug PTFE 63865

3 Adapter Luer cone PTFE 63863


only for pressures up to 0.4 bar rel.
1 Adapter UNF ¼" Luer male 64793

2 Adapter Luer ¼" UNF 64792


(only in accessory kit DMA 5000 M)

3 Hose clamp 21531

2 Pan head screws M3x16 66750

1 Phillips screwdriver PH-0x40 75030

12 XDLIB016EN-K
3 Checking the Supplied Parts

Table 2: Optional accessories and consumables

Article description Mat. no.


Data handling
Keyboard German USB 80809
Keyboard USA USB 80807
Printer RS-232C incl. cable 9600N81 44737
Printer Epson TM-U220D or B 93362
RS-232 connection cable D-Sub 9-pin, 3 m 70429
Gender changer DB9M/DB9M 302592
Automatization
Xsample 320 184368
Xsample 330 184372
Xsample 340 with Cleaning 164758
Xsample 520 incl. 48 pos. / 12 mL magazine 184346
Xsample 520 incl. 24 pos. / 50 mL magazine 184345
Xsample 530 incl. 71 pos. / 12 mL magazine 165604
Xsample 530 incl. 35 pos. / 45 mL magazine 165605
Protection
Protecting cover for keyboard 13350
Protection cap for USB interfaces 156194
Special funnel protection 82448
Special application accessories
Aerosol Adapter 74650
Drying cartridge (with silica gel) 65085
Heating attachment for DMA M 83161
Syringes
Syringe 2 mL Luer (1 pc.) 51974
Syringes 2 mL Luer (10 pcs.) 58802
Syringes 2 mL Luer (1000 pcs.) 66399
Syringes 5 mL Luer (100 pcs.) 6772

XDLIB016EN-K 13
4 Installing the Instrument

4 Installing the Instrument


To install the instrument, put it on a bench, mount
injection adapters and hoses, and connect the
4.2 Mounting the Injection Adapters
instrument to the AC power supply. Define general
1. Take two injection adapters with screws from
instrument settings and perform an air/water check
the accessory kit.
to check the validity of the factory adjustment.
2. Pull the black plastic transport plugs out of the
For the installation of an Xsample filling module, see injection adapters’ tips.
the manual of the Xsample.
TIP: Keep the transport plugs for later use. In case
of leaks you can widen the tips of the adapters with
4.1 Installation Requirements the transport plugs.

The instrument is designed for operation under


typical laboratory bench top conditions.

WARNING
Using hazardous or flammable chemicals as
samples or cleaning liquids could lead to damage
of the instrument and cause serious injuries
unless special precautions are taken.
• Observe the safety instructions in section 1.

Place the instrument on a stable, flat bench that is


free from vibrations and away from vibrating equip-
Fig. 5: Mounting the injection adapters
ment.
To ensure temperature stability and trouble-free 3. Carefully insert the injection adapters into the
measurement, do not position your instrument: openings of the adapter holding plate on the
right side of the instrument, see fig. 5.
- next to a heating facility,
4. Push both adapters towards the adapter holding
- in a drafty place (e.g. near an air conditioning,
plate with moderate force.
ventilation system, or an open window),
- in direct sunlight. 5. Insert the screws through the bore holes of the
adapters and screw them cautiously into the
adapter holding plate until some resistance
NOTICE
against further turning can be felt.
• Ensure that the power plug and the power
switch are always easily accessible so that the
instrument can be easily disconnected from the
AC power supply at any time. CAUTION
• A strong built-in cooling fan dissipates heat
through the bottom and the rear of the instru- If the screw for fastening the adapter is over-
ment. Ensure that the air flow is not blocked, tightened, the density measuring cell may get
and provide for a minimum distance of 10 cm damaged. Harmful liquids leaking from the
(4 in) to walls behind and beside the instru- instrument may cause injuries.
ment. • Tighten the screw until some resistance against
• High humidity or a measuring temperature that further turning can be felt, and then stop to
is significantly below the ambient temperature tighten the screw.
may lead to condensation in the measuring cell. The gap left between the holding plate and the
Install a drying cartridge to avoid condensation, adapter, where the thread of the screw can be
see section 8.8. seen, is approx. 3–8 mm (approx. 0.12–0.31 in).

14 XDLIB016EN-K
4 Installing the Instrument

4.3 Leak Tightness Test DMA 4100/4500 M: Connecting the waste


vessel by a silicone hose
1. For DMA 5000 M: Insert the adapters Luer ¼"
1. Screw an adapter UNF ¼" Luer, mat. no. 64793
UNF into the openings of the injection adapters.
(from the accessory kit), into the threaded hole
2. Close one adapter tightly with a male Luer plug. in the cap of the waste vessel.
3. Use a plastic syringe from the accessory kit to 2. Cut a piece of approx. 25 cm (10 in) length from
inject, with moderate pressure, air through the the supplied silicone hose 4x6, mat. no. 57024.
other adapter.
3. Connect one end of the silicone hose to the
4. Wait a few seconds, then release the plunger of adapter UNF ¼" Luer and fix it with a hose
the syringe. clamp (from the accessory kit).
- If the connections are tight, the plunger of 4. Attach an adapter Luer cone PTFE, mat. no.
the syringe will be slowly pushed back by the 63863 (from the accessory kit), to the other end
pressure in the measuring cell. of the silicone hose and fix it with a hose clamp
- If the connections are leaky, the plunger of (from the accessory kit), see fig. 6.
the syringe will not move.
5. Insert it into the rear injection adapter of DMA M.
In this case, remount the adapters.
TIP: In case of leaks you can widen the tips of the
adapters with the transport plugs of the adapters.

4.4 Mounting the Hoses

WARNING
Liquids leaking from the instrument may cause
injuries or risk of fire.
• Only use the supplied hose and waste vessel if
their materials are resistant to the samples and
cleaning liquids that you are going to inject.
• If the supplied parts are not suitable, use other
parts made of an appropriate material.
Fig. 6: Connecting the waste vessel hose

Connecting the air pump hose (silicone)


DMA 5000 M: Connecting the waste
1. Cut a piece of approx. 35 cm (14 in) length from vessel by a PTFE hose
the supplied silicone hose 4x6, mat. no. 57024.
1. Screw one end of the hose 300x3x2 PTFE, mat.
2. Connect one end of the hose piece to the air
no. 3443 (from the accessory kit DMA 5000 M),
pump outlet.
into the threaded hole in the cap of the waste
3. Attach an adapter Luer cone PTFE, mat. no. vessel, see fig. 7.
63863 (from the accessory kit), to the open end
2. Screw the other end of the hose into the rear
of the hose piece.
injection adapter.

XDLIB016EN-K 15
4 Installing the Instrument

DMA 5000 M: Connecting the filling hose 4.6 Power Connection


1. Screw an adapter Luer ¼" UNF, mat. no. 64792
(from the accessory kit DMA 5000 M), into the
upper screw hole of the syringe holder.
WARNING
2. Screw one end of the hose 140x3x2 PTFE,
mat. no. 187223 (from the accessory kit High voltage at parts of the instrument can
DMA 5000 M), into the lower screw hole of the cause serious injuries or death
syringe holder. • Connect the instrument only to an electrical
3. Screw the other end of the hose into the front outlet with protective earthing.
injection adapter, see fig. 7. • Never connect the instrument to the AC power
supply with protective separation or protective
insulation.
• Ensure that the non-fused earth conductor of
the power cable is connected to earth.

NOTICE
Possible damage due to wrong voltage
Before you switch on the instrument, make sure
that the correct line voltage and line frequency
are available (AC 100–240 V, 50/60 Hz).
If large voltage fluctuations are to be expected,
Fig. 7: PTFE hoses mounted on DMA 5000 M
we recommend using a constant voltage source
(UPS).
4.5 Connecting the Cooling • Connect the AC power jack of the instrument
(only for DMA CK versions) (10, fig. 4) to a suitable electrical outlet with the
supplied power cable.
When you perform measurements at temperatures
lower than 20 °C (36 °F) below ambient tempera-
ture, connect the cooling to an external thermostat.
If your tap water is cool enough, also connecting to
4.7 Switching the Instrument On/Off
a tap water supply will help. Operate the cooling with
• Use the power switch on the rear of the instru-
a moderate flow of water (1 to 3 liters per minute).
ment (8, fig. 4) to switch the instrument on or
off.
temperature range of
5–30 °C (41–86 °F) The green LED on the front of the instrument
the cooling unit
(1, fig. 2) indicates that the power is on.
maximum pressure 1 bar (14.5 psi) relative
• After power-on wait at least 15 minutes for the
self-locking coupling
internal temperature to stabilize.
8 mm, type Rectus
connector During the time that the instrument needs for
21KBTS08MVN,
mat. no. 75090 temperature equilibration and internal tempera-
ture adjustments, “temp. equilibration” is dis-
played.
Example
TIP: Do not turn off the instrument during the night.
Your ambient temperature is 25 °C (77 °F), and you
This allows the measuring cell to achieve long term
want to perform measurements at 0 °C (32 °F).
temperature stability.
• Connect the DMA M CK to an external thermo-
stat or a tap water line delivering water at a IMPORTANT: If you have to restart the instrument,
constant temperature between 5 °C and 15 °C switch it off and wait until the green LED on the front
(41 °F...59 °F), and set the measuring tempera- has gone out before switching the instrument on
ture to 0 °C (32 °F) in the “Density Module” again.
dialog.

16 XDLIB016EN-K
4 Installing the Instrument

4.8 Basic Instrument Settings / To perform first checks


First Checks IMPORTANT: Wait at least 15 minutes after a
restart for the internal temperature to stabilize.
After hardware installation set the date and time, see 1. To perform an air check, tap <Menu> and select
General Software Functions Manual, section 6.1.1. Checks/Adjustments > Checks. Proceed as
To check the validity of the factory adjustment, described in section 9.2.2.
perform an air check and a water check. 2. To perform a water check, tap <Menu> and
select Checks/Adjustments > Checks. Proceed
The instrument has been factory adjusted over the
as described in section 9.2.2.
whole temperature and viscosity range, but during
transport the density adjustment may have been If both checks succeed, your instrument is ready for
compromised. routine measurements.
- If a check fails, clean the measuring cell
thoroughly and repeat the check.
- If the check still fails, perform an air/water
adjustment as described in section 9.3.1.

XDLIB016EN-K 17
5 Operating the Instrument

5 Operating the Instrument


5.1 Operating Elements on the Main Screen
1

3 6

IMPORTANT: Corresponding
with your user group rights (see
4
the General Software Functions
5 Manual, section 6.5.1), operating
elements may be locked.

Fig. 8: Example main screen

1 Header 4 Status bar


2 Output field 5 Buttons area
3 Contents area 6 Quick access area

Header Measuring mode


On the left of the header you find the name of the If you have started a measurement, a continuous
currently active method and the sample name. reading of the current measuring values is shown
until the measurement is finished. The final values
On the right of the header you find a clock and the
stay frozen on the screen until the next measure-
user indicator. The user indicator indicates the type
ment is started. To unfreeze the screen and change
of user that is currently logged in.
to monitor mode, tap in the quick access area.

Contents area Buttons area


In the contents area the measuring values are
The buttons on the main screen have the following
displayed in small, medium, or large output fields.
functions:
The layout of the contents area can be defined in the
settings of the current method according to your
needs. Button Function

The status bar at the bottom of the contents area <Menu> Opens the main menu.
shows the status of the instrument or a measure- <Quick Settings> Opens the quick settings list
ment. If applicable, a progress bar shows the prog- (only available in the “No
ress of activities. Sample List” mode instead of
the <Sample List> button).
Monitor mode <Sample List> Opens the current sample list.
If you have not started a measurement yet, or if you <Method> Opens the method list
have terminated a measurement by tapping <Stop>, (to select a method).
the instrument is in the monitor mode and shows a <Start> Starts a measurement.
continuous reading of the current measuring values. <Stop> Stops and aborts a measure-
ment.

18 XDLIB016EN-K
5 Operating the Instrument

Quick access area


Function
Opens the message list.
The general instrument status as well as all
measuring errors that have occurred during
the measurements of the currently active
sample list are described in this list. The
button changes its appearance depending
on the current error status:
• Green OK sign:
The general instrument status and the
error status of all measured samples of
the current sample list are OK.
• Yellow warning sign:
- The instrument (or system) has a minor
problem (e.g. an air or custom check is
Fig. 9: Expanded quick access area overdue, there is a printer problem etc.).
- There has been a filling error with one
• To expand the quick access area, tap on
or more samples of the currently active
the quick access bar.
sample list.
• To collapse the quick access area, tap in
• Red error sign:
the upper right corner of the expanded quick
- The instrument (or system) has a major
access area.
problem that needs to be fixed before
• To browse items, use the page navigation you continue with measurements
in the header of the expanded (e.g. the sample changer is blocked).
quick access area. - One or more samples of the current
• To rearrange the items in the quick access sample list could not be measured
area, tap (settings) in the upper left corner (e.g. the measuring cell is partly empty
of the expanded quick access area. For details so that it cannot oscillate).
see the General Software Functions Manual, To reset the message list button to the
section 4.8. green OK sign, confirm all error messages
by tapping on the <X> button on the right of
the message. To confirm all messages in
the list in one step, tap “Delete all” at the
end of the list.
The message list button will also be reset
to the green OK sign if you delete the
currently active sample list, see General
Software Functions Manual, section 7.6.
U-View™: Opens the live camera view of
the measuring cell.
Starts/stops the air pump.
The air pump is off.

The air pump is on.

Unfreezes the screen after a finished


measurement.
The screen is frozen.
The screen is unfrozen. A continuous
reading of the current measuring values is
shown.

Displays information on using favorites.

XDLIB016EN-K 19
5 Operating the Instrument

5.2 Operating Elements on the Menu Screen


To access the menu, tap <Menu> on the main screen.

A1

A2

A5

A3
IMPORTANT: Corresponding
with your user group rights (see
the General Software Functions
A4
Manual, section 6.5.1), operating
elements may be missing.
B1

B3

B2

Fig. 10: Example menu screens

A1 Header B1 <Add to Favorites> button


A2 Menu level 1 B2 Buttons area
A3 <Back> button B3 Contents area
A4 <Home> button
A5 Contents area

Header Buttons area


On the left of the header you find the navigation path The buttons on menu screens have the following
to your current position in the menu. You can go functions:
back to any menu position in your current path by
directly tapping on the respective box of the naviga- Button Function
tion path. For details on using the <Add to Favor-
ites> button, see the General Software Functions <Back> Moves to the next higher
Manual, section 4.8. menu level.
<Home> Returns to the main screen.
Contents area Buttons at the Functions depending on the
bottom of screens current menu or dialog
In the contents area you find the menu options of the
current menu level and the menu dialogs.

20 XDLIB016EN-K
6 Camera Settings

6 Camera Settings
6.1 Adjusting the Camera Position 6.2 Setting the Camera Illumination
If the camera does not show the complete measur- You can adjust the illumination of the camera picture
ing cell, you can adjust the position of the camera. to suit your environment.
1. Tap in the quick access area. 1. Log in as “administrator”.
The camera window opens. 2. Tap <Menu> and select Setup > Control Panel
> Advanced Camera Settings.
3. Change the value “Auto Exposure Luminance”
to adjust the brightness of the camera picture.

6.3 Saving a Camera Picture


You can specify that the instrument shall automati-
cally save a picture of the measuring cell.
1. Tap <Menu> and select Setup > Measuring
System Settings > Camera.
2. Use the radio buttons to select one of the
Position buttons options:
Automatically save a picture …
Fig. 11: Adjusting the camera position
- of each measurement
2. Use the position buttons to adjust the position - only if there is a filling warning
of the camera. - never
3. Close the camera window by tapping <X>. 3. Tap <OK> to save the changes.

XDLIB016EN-K 21
7 Defining and Using Methods

7 Defining and Using Methods


7.1 Measuring Methods Factory preset methods
The instrument comes with a set of 10 predefined
Each method contains the following kind of informa- methods covering the most common applications.
tion:
The measuring temperature for these 10 methods is
- Instrument settings set to 20 °C.
- Xsample settings and measuring module
settings (if any module is installed)
- Layout of measuring data on the main screen
- Measuring units
- Parameter list for printout and data export
You can use the factory preset methods as they are
or change them to suit your needs. You can also
create new methods. For details see the General
Software Functions Manual, section 7.2 and
section 7.3.

Fig. 12: Example: Measurement with method “Density”

• General purpose method


Density • Output fields: Density, Specific Gravity, Density Temperature, Density Condition,
U-View™
• General purpose method, for comparison with old instruments without viscosity
Density correction
(not visc.-corr.) • Output fields: Density (not visc.-corr.), Specific Gravity (not visc.-corr.), Density
Temperature, Density Condition, U-View™
• For measurements of sugar in soft drinks
°Brix • Output fields: Concentration Sugar, Density, Density Temperature, Density
Condition, U-View™
• For measurements of alcohol concentration in distillates
Ethanol
• Output fields: Ethanol OIML-ITS-90 (% w/w), Density, Density Temperature,
(% w/w OIML-ITS-90)
Density Condition, U-View™
• For measurements of alcohol concentration in distillates
Ethanol
• Output fields: Ethanol OIML-ITS-90 (% v/v), Density, Density Temperature,
(% v/v OIML-ITS-90)
Density Condition, U-View™
• For measurements of alcohol concentration in distillates
Ethanol
• Output fields: Ethanol Proof 60 °F, Density, Density Temperature, Density
(°Proof 60 °F AOAC)
Condition, U-View™
• For measurements of crude oil according to calculations for product group A with
temperature correction to 15 °C
Crude Oil (API)
• Output fields: API Density 15 °C, Density, API Specific Gravity 15 °C, Density
Temperature, °API Gravity 15 °C, Density Condition, U-View™
• For measurements of fuel oil according to calculations for product group B with
temperature correction to 15 °C
Fuel Oil (API)
• Output fields: API Density 15 °C, Density, API Specific Gravity 15 °C, Density
Temperature, °API Gravity 15 °C, Density Condition, U-View™

22 XDLIB016EN-K
7 Defining and Using Methods

• For measurements of lubricants according to calculations for product group D


with temperature correction to 15 °C
Lubricants (API)
• Output fields: API Density 15 °C, Density, API Specific Gravity 15 °C, Density
Temperature, °API Gravity 15 °C, Density Condition, U-View™
• For measurements of sulfuric acid up to 94 % w/w
Sulfuric Acid
• Output fields: Sulfuric Acid (H2SO4) (% w/w), Sulfuric Acid (H2SO4) (mol/L),
(% w/w)
Density, Density Temperature, Density Condition, U-View™

7.2 Changing Methods reached precision class, see appendix B. In this


case, we recommend deactivating the function
“Density stability criterion”.
You need administrator rights to create, edit, or
delete methods. The maximum number of methods
is 400. Temperature
For setting the displayed output fields, result output Measuring temperature
quantities, limits and quick settings parameters, see
the General Software Functions Manual, Timeout
section 7.2.
If a measurement is not finished after the specified
timeout, it will be aborted. The timeout count starts
7.2.1 Measurement Settings of the when temperature equilibrium is reached.
Density Module
FillingCheck™
Precision class FillingCheck™ automatically detects inhomogene-
DMA M provides the following precision classes: ities and gas bubbles in the whole measuring cell by
an advanced analysis of U-tube's oscillation pattern.
- Ultrafast If applicable, it will generate a warning message in
- Fast real time for each single measurement.
- Standard
- Precise (only with DMA 5000 M)
Measurement delay
By default, each precision class has defined stability
and repeatability criteria for temperature equilibra- The instrument postpones the finish of the measure-
tion, see table 10 in appendix A.1 for the stability ment for the defined time after reaching the set
criteria of each precision class. precision class.

If the check box “Density stability criterion” is acti- Viscosity correction


vated additionally, the defined stability and repeat-
ability criteria for density are also checked. For each method you can set one of three viscosity
correction modes and define, whether the viscosity
A measurement is valid, if the fluctuations of tem-
correction shall be applied automatically, manually,
perature and density (if activated) over time fulfill the
or not at all.
stability criteria of the set precision class.
With automatic viscosity correction:
If you select “Ultrafast”, the instrument finishes the
measurement before temperature equilibrium has The viscosity correction works best for Newto-
been reached, and calculates the density at the set nian fluids. If samples have a non-Newtonian
temperature in advance (extrapolation of the density behavior (e.g. due to the presence of significant
at the set temperature). This saves time, but makes particle concentrations), the viscosity correction
the result less accurate. may deliver less accurate results.

If DMA M cannot meet the criteria for the set preci- With manual viscosity correction:
sion class (e.g. due to the presence of air bubbles or - If the viscosity of the sample is known (e.g.
particles), it will display a timeout error. The output from a certificate of a CRM or from a mea-
quantity “Stability status” indicates the actually surement with a viscometer), the viscosity of
the sample can be entered in the mandatory

XDLIB016EN-K 23
7 Defining and Using Methods

input field “Set viscosity” when you start a Table 3: Measurement modes (cont.)
measurement. Or it can be entered in the for-
mula parameters of the method settings. RM (Repeated Mode) to perform repeated mea-
- The entered viscosity has to be valid for the surements of a single
measuring conditions (e.g. temperature) of sample by filling the
the density measurement. sample up to 5 times and
- The entered viscosity has to be correct. defining a maximum devi-
False viscosity values may lead to a filling ation of two subsequent
warning. measurements
- In the continuous monitor mode, the viscos- MF (Multiple Filling) to perform multiple mea-
ity-corrected density is not available. surements of a single
sample by filling the
sample 2 to 10 times
7.2.2 Defining Measurement Settings
TS (Temperature to perform a temperature
To define the measurement settings described in Scan) scan
section 7.2.1, proceed as follows:
TTS (Temperature to perform a temperature
1. Tap <Menu> and select Methods > Method Table Scan) table scan
Settings > method name > Density Module.
2. Define the following settings: TIP: The exported PDF file of measurements in the
- Enter the measuring temperature. MM, RM, or MF mode also includes the arithmetic
- Define the timeout. mean and the standard deviation of each multiple
- Select an option for the FillingCheck™ measurement series. The standard deviation is
(always active, not active, active during calculated according to the following formula:
measurement).
- Define a measurement delay for the finish of n n 2
2
the measurement (default 0 s, max. 600 s). n  i=1
 xi  –  i=1
xi
3. Tap <Next>. sd = ------------------------------------------------------------------------------
n  n – 1
4. Define the following settings:
sd ..... empirical standard deviation
- Select the precision class (default: Standard).
n ....... number of measurements in the series
- Activate/deactivate the check box “Density xi ....... measured value of the ith measurement
stability criterion”.
5. Tap <OK>. “Standard” mode
1. Tap <Menu> and select Methods > Method
7.2.3 Defining the Measurement Mode Settings > method name > Measurement Mode.
For each method, you can set one of the following 2. To select “S (Standard)”, highlight the item and
measurement modes: tap <OK>.

Table 3: Measurement modes “Check” mode


S (Standard) to perform a standard Air Check and Water Check are predefined for all
measurement methods. User-defined checks are only available
with the method that has been assigned to the
C (Check) to perform one of the check.
predefined checks
1. Tap <Menu> and select Methods > Method
MM (Multiple to perform 2 to 10 mea- Settings > method name > Measurement Mode.
Measurements) surements of a single
sample automatically 2. To select “C (Check)”, highlight the item and tap
<Next>.
3. Select one of the defined checks and tap <OK>.

24 XDLIB016EN-K
7 Defining and Using Methods

“Multiple Measurements” mode (If the deviation criteria cannot be met because
the results of the single determinations differ
Using multiple measurements enables you to per- too much, the result of each determination and
form several measurements automatically. A single the mean of the results will be saved.)
entry in the sample list starts a series of up to 10
4. Select the “Avg. Calculation Mode”: Define how
measurements of a sample and calculates the aver-
the mean shall be calculated.
age values of these measurements.
- “Standard”: The mean is calculated based
Multiple measurements create additional entries in on the results of all determinations.
the data memory as not only the single measure- - “ASTM D4052 compliance for opaque
ments, but also the average values are calculated samples”: The mean is calculated based on
and stored. the two highest density results of the valid
1. Tap <Menu> and select Methods > Method determinations.
Settings > method name > Measurement Mode. If you select “ASTM D4052 compliance for
opaque samples”, an additional deviation
2. To select “MM (Multiple Measurements)”, high-
criterion, “Max. allowed diff. between valid
light the item and tap <Next>.
two samples”, is shown and has to be
3. Select the number of multiple measurement defined (in g/cm3).
cycles and tap <OK>. In case a measurement cannot find valid
determinations that meet this additional
“Repeated Mode” criterion:
- A yellow warning sign in the quick access
Using repeated mode enables you to perform up to area will show.
5 filling procedures and subsequent measurements - A message in the “Message List” window
(determinations) from the same syringe or sample will warn you.
vial without cleaning in between. You can use the output quantity “Sample
1. Tap <Menu> and select Methods > Method Error State” in the result output to report the
Settings > method name > Measurement Mode. status with the measurement data.
2. To select “RM (Repeated Mode)”, highlight the 5. Tap <Next>.
item and tap <OK>. 6. Activate/deactivate the quantity for which the
The various settings for the repeated mode have to deviation criterion shall be tested.
be set separately under “Repeated Mode Settings”. If activated, the deviation between two subse-
quent determinations is calculated and com-
Repeated mode settings pared with the “Max. Repeat Value”. If the
deviation is less than this value, the determined
1. Tap <Menu> and select Methods > Method results are considered valid, and the measure-
Settings > method name > Repeated Mode ment is finished.
Settings. 7. Use the default maximum deviation value for
2. Select “Max. Number of Determinations”: The the selected quantity or deactivate the check
instrument tries to determine measuring values box “Use Default” and enter your own “Max.
that fulfill the deviation criteria defined below. If Repeat Value” (table 5 gives the allowed range
such values cannot be found (or if the criteria are for density).
not tested), the measurement is finished after
Table 4: Default maximum density deviation values
the set maximum number of determinations has
been reached. Deviation [g/cm3]
3. Select the “Save Mode”: Define which measure- DMA DMA DMA
ment results shall be saved in the data memory. Precision class
4100 M 4500 M 5000 M
- “All”: The results of all single determinations Ultrafast 0.0003 0.00005 0.000005
and the mean of the results are saved.
Fast 0.0001 0.00001 0.000003
- “Valid Two Only”: Only the results of the two
determinations that fulfill the deviation criteria Standard 0.0001 0.00001 0.000002
and the mean of these are saved. Precise – – 0.000001
- “Final One Only”: Only the result of the final
determination that fulfills the deviation criteria
and the corresponding mean are saved.

XDLIB016EN-K 25
7 Defining and Using Methods

Table 5: Range of maximum density deviation values


Minimum
Precision class Model
Deviation DMA DMA DMA step size
[g/cm3] 4100 M 4500 M 5000 M Ultrafast 1 °C all models
Minimum 0.0001 0.00001 0.000001 Fast 0.1 °C all models
Maximum 0.001 0.001 0.001 Standard 0.01 °C all models
Precise 0.005 °C DMA 5000 M
8. Tap <OK>.
TIP: To view and save the deviation between two Set the temperature step interval so that the instru-
valid determinations, select the output quantity ment can reach the end temperature by a whole
“Repeat Deviation Density” for the display layout number of steps (divide the interval between start
and result output. and end temperature only by whole numbers to find
appropriate step settings).
“Multiple Filling” mode TIP: To ensure highest precision of the measure-
ments, set a measurement delay time of at least
Using multiple filling enables you to perform mea-
2 minutes.
surements of a single sample by refilling the sample
up to 10 times. If multiple filling measurement is per- 1. Tap <Menu> and select Methods > Method
formed, an additional entry in the data memory is Settings > method name > Measurement Mode.
created as not only the single measurements, but 2. To select “TS (Temperature Scan)”, highlight
also the average value is calculated and stored. the item and tap <Next>.
1. Tap <Menu> and select Methods > Method 3. Enter the “Start”, “Step” and “End” temperature
Settings > method name > Measurement Mode. of the temperature scan.
2. To select “MF (Multiple Filling)”, highlight the The start temperature has to be higher than the
item and tap <Next>. end temperature to prevent degassing in the
3. Use the “Multiple filling” drop-down box to measuring cell.
select the number of measurements (up to 10). 4. Tap <OK>.
4. Tap <OK>.
“Temperature Table Scan” mode
“Temperature Scan” mode Using temperature table scan measurements
Using temperature scan measurements enables enables you to perform measurements of a sample
you to perform measurements of a sample at at several defined temperatures.
several temperatures that are defined by intervals in Temperatures from 0 °C to 100 °C are allowed.
a set temperature range.
For the minimum difference between two consecu-
Temperatures from 0 °C to 100 °C are allowed. tive temperatures, see the table listing the minimum
step sizes for the temperature scan mode.
TIP: To ensure highest precision of the measure-
WARNING ments, set a measurement delay time of at least
2 minutes.
Liquids leaking from the instrument may cause
injuries and risk of fire. 1. Tap <Menu> and select Methods > Method
• When performing temperature scans or tem- Settings > method name > Measurement Mode.
perature table scans, make sure that the wetted 2. To select “TTS (Temperature Table Scan)”,
parts are resistant to the filled-in liquid at all highlight the item and tap <Next>.
measuring temperatures (see appendix A.3).
3. Enter the desired temperature values in the
table, and tap <OK> after each entry.
The minimum step size between two consecutive
temperatures depends on the precision class of the The start temperature has to be higher than the
density module, see the table below. end temperature to prevent degassing in the
measuring cell.
4. Activate or deactivate repeated mode for each
temperature value in the list.

26 XDLIB016EN-K
7 Defining and Using Methods

The various settings for the repeated mode Parameter “Density API Alpha Factor”
have to be set separately under “Repeated
Mode Settings”. For liquids that are assigned to the special applica-
tions category, a specific thermal expansion coeffi-
IMPORTANT: When using temperature table scan cient has to be established for each particular liquid.
with repeated mode, the calculations for
“Measurement Mode Functions” and “ASTM D4052
compliance for opaque samples” might not work
Parameter “Density Canadian Excise
with DMA 4100/4500/5000 M instruments. Alcohol Table”
5. Tap <OK> to save the settings. The input quantity for the Canadian Excise Alcohol
Table can be defined as:

7.2.4 Defining Formula Parameters - Special Adjustment 1, …, 5


see section 9.3.4.2
You can enter formula parameters to define how
API parameters shall be determined and to define Parameter “Density Set Viscosity”
which special adjustment shall be used for the
Canadian excise alcohol table. Only available if the method is using the viscosity
correction mode “Manual viscosity input”. The
viscosity of the sample has to be entered in mPa·s.
Parameter “Density API Input Quantity”
API parameters are usually calculated based on To define formula parameters
true density; the input quantity can be defined as:
1. Tap <Menu> and select Methods > Method
- Density (not visc.-corr.) Settings > method name > Formula Parameters.
- Density
2. Select/specify the required parameters:
- Special Adjustment 1, …, 5
- Select an API Product Group and an API
Input Quantity.
Parameter “Density API Product Group”
- Or select the special adjustment for the
The API Product Group can be set to A (crude oil), Canadian Excise Alcohol Table.
B (fuels), or D (lubes) to set up measuring methods 3. Tap <OK>.
for different product groups. You can also define an
API Product Group of your own (Custom) for special TIP: Before you use the output quantity “Canadian
applications. Excise Alcohol Table” of the group “Ethanol Tables”
(see appendix B), it is necessary to perform a
The conversion formulas from input quantities special adjustment with apparent density values of
(Density etc.) to API quantities differ between the air and water (see section 9.3.4.2) and link that
product groups and therefore need to be defined for adjustment to the Canadian Excise Alcohol Table.
the measuring methods.

XDLIB016EN-K 27
8 Performing a Measurement

8 Performing a Measurement
8.1 Sample Name
WARNING If you have defined automatic sample name parts
(see General Software Functions Manual,
Risk of injuries or fire caused by hot liquids
section 6.3), they will be added to each sample
spurting out of the measuring cell
name after the measurement has finished.
In the unlikely case of a malfunction or damage
of the Peltier elements, the heating control of the The complete sample name, including automatic
measuring cell is affected, and the temperature sample name parts, can be up to 50 characters long.
of the measuring cell might rise up to 120 °C
(248 °F) (for DMA M with DSP-SAC electronics,
up to 150 °C/302 °F). 8.2 Filling Samples
To avoid injuries and fire:
• Ensure that the waste vessel is properly To achieve highly accurate measuring results, fill
installed. the sample into the measuring cell steadily and
• Use method settings that constantly display the without bubbles.
temperature of the measuring cell.
IMPORTANT: For high accuracy measurements:
• Check the temperature of the measuring cell
• Be sure to apply exactly the same filling procedure
before you fill a sample or start a measurement.
for checks, adjustments, and measurements.
• If you measure aggressive, toxic, or flammable
• If you use a syringe for filling, use the syringe
samples, use only the smallest possible sample
holder to fully utilize the instrument’s accuracy
amount.
(especially with DMA 5000 M). Inject the entire
• If your sample is toxic or highly flammable,
sample volume. The syringe can stay connected
always handle it in an appropriate environment,
to the filling adapter during the measurement.
e.g. under a fume hood, and ensure that the
location is sufficiently ventilated.
• Measure only samples with an ignition point
over 120 °C (248 °F) (for DMA M with DSP- WARNING
SAC electronics, over 150 °C/302 °F).
• Wear protective clothing, and safety goggles. Filling samples or cleaning liquids that the wetted
parts are not resistant to will corrode the wetted
parts. Sample leaking from corroded parts may
Preparatory steps cause serious injuries.
Before you start a measurement, check that: Before you fill any sample or cleaning liquid into
the instrument:
- the measuring cell is clean and dry,
• Make sure that all safety instructions concern-
- hoses are connected correctly,
ing the use of chemicals and the use of flamma-
- hose connections are tight,
ble chemicals are met, see section 1.
- the waste hose leads into the waste container,
• Make sure that all wetted parts are resistant to
- the volume of the waste container is large
the filled-in liquid, see appendix A.3. The chem-
enough for the number of samples,
ical resistance depends on the temperature and
- the correct sample names are entered,
concentration of the sample.
- the method settings are set correctly,
Consider also the wetted parts of an optionally
- suitable cleaning liquids are at hand.
installed Xsample filling module (refer to the
manual of the Xsample).
To speed up measurements • Make sure that suitable cleaning liquids for
• Use automatic sample naming (see General cleaning the measuring cell are at hand, see
Software Functions Manual, section 6.3). section 10.1.
• Bring the sample to measuring temperature in
advance to reduce the time necessary for the
temperature equilibration.
• Using precision class “Ultrafast” reduces the
measuring time significantly, see section 7.2.1.

28 XDLIB016EN-K
8 Performing a Measurement

To fill with a syringe (Luer tip)


NOTICE
Corrosive samples require special care IMPORTANT: Do not use syringes that contain
Samples with a moderate tendency to corrode lubricants. The lubricants can dissolve into your
borosilicate glass, such as strong alkali solutions sample and lead to a systematic measuring error.
(e.g. caustic soda), can be measured with the
DMA M. However:
• Remove corrosive samples immediately after
measurement and rinse the measuring cell
thoroughly.
• Check the validity of the adjustment more
frequently than generally recommended.
Perform a new adjustment if necessary.
• The measuring temperature for strong alkali
solutions should not be higher than 20 °C
(68 °F). Higher temperatures dramatically
increase the speed of corrosion.
Fig. 14: Filling with a syringe

Sample amount 1. Connect the syringe to the sample inlet adapter


or to the adapter Luer ¼" UNF, mat. no. 64792,
If the measuring cell is clean and dry, you need
in the top connector of the syringe holder, see
approx. 1 mL of sample.
fig. 14.
If you measure without cleaning and drying between 2. Push the plunger of the syringe slowly and
samples, you will need a higher amount of sample steadily until a drop emerges from the sample
because you have to flush residues of the previous outlet adapter.
sample out of the measuring cell to avoid cross-
contamination. 3. Leave the syringe in the filling position during
the measurement.
Bubble detection using the camera –
To fill with a funnel
U-View™
1. Attach an adapter Luer cone PTFE, mat. no.
• Tap in the quick access area to open the
63863, to the sample inlet adapter.
live camera view of the measuring cell.
2. Connect a funnel to the adapter by a silicone
- Tap <Zoom In> to get a magnified view.
hose 3x5.
- Attach a USB memory device and tap <Save
Picture> to save the current picture. 3. Fix the funnel in a position higher than the
sample inlet of the DMA M.
• Tap <X> to exit the measuring cell view.
4. Attach another adapter Luer cone PTFE, mat.
no. 63863, to the sample outlet adapter.
5. Connect a waste vessel to the adapter by
another silicone hose 3x5.
6. Mount a valve or hose clamp at the outlet
silicone hose.
7. Close the valve and fill your sample into the
funnel.
8. Fill the measuring cell by carefully opening the
valve and closing it again before the funnel runs
empty.
Fig. 13: Camera window

XDLIB016EN-K 29
8 Performing a Measurement

To fill with a peristaltic pump of valid (black) digits will increase during mea-
surement progress until all digits are black
(depending on the set precision class).
NOTICE
• The liquid levels in the sample container and When the measurement is finished, the prog-
the waste vessel must be below the filling level ress bar turns green, the message “Finished” is
of the instrument. Never put the peristaltic displayed, and an acoustic signal is given. The
pump or the waste vessel on top of the instru- output field “Density Condition” shows the
ment. status “valid”. The result values are saved in
• Check the hoses of the peristaltic pump daily. the data memory and can be viewed, printed,
• Check the life time of the hoses specified by the exported or deleted.
supplier, and change the hose frequently. The result values on the screen are frozen. Tap
in the quick access area to unfreeze the
1. Attach an adapter Luer cone PTFE, mat. no. screen..
63863, to the sample inlet adapter.
2. Connect the sample container to the adapter by
a silicone hose 3x5.
8.4 Filling and Measurement
3. Attach another adapter Luer cone PTFE, mat. Warnings
no. 63863, to the sample outlet adapter.
4. Connect another silicone hose 3x5 to the outlet 8.4.1 Status Messages
adapter Luer cone and lead it through the
peristaltic pump into a waste vessel. Density condition
5. Set the flow rate of the pump to 10–25 mL/min.
The output field “Density Condition” gives informa-
6. Start the pump. tion about the current status of the measurement:
7. Turn off the pump after filling a sufficient amount Table 6: Density condition status
of sample.
temp. Appears during temperature equili-
To fill automatically with an Xsample equilibration bration. In this stage no predeter-
mined result can be determined by
For details see the manual of the Xsample. the instrument.
acquisition Appears after the temperature
equilibration has reached the tem-
8.3 Measurement Procedure perature stability of the precision
class “Ultrafast”.
Proceed by the following steps:
pre- Appears before the exact measur-
- Select a method.
determined ing temperature has been reached
- Fill the sample.
and when the instrument can deter-
- Perform the measurement.
mine a predetermined result.

To perform a measurement valid Appears when the measuring tem-


perature has been reached and
1. Enter a sample name if required (see also the measurement has been taken.
section 8.1).
2. Tap <Start> and wait until the measurement is Sample status icons
finished.
In the first column of the sample list, you find an icon
The progress bar shows the progress of the for each sample that has already been measured.
measurement by a growing red bar and the The icon indicates the status of the sample:
message “Measuring” or “Measuring (delayed)”
if a measurement delay time has been set (see
The sample has been successfully measured
section 7.2.1).
During measurements, the last 1, 2, or 3 digits Reduced precision due to e.g. a filling error
may be grayed signifying that the set tempera- No result due to a malfunction
ture has not been reached yet. In this case,
only the solid black digits are valid. The number The measurement has been canceled

30 XDLIB016EN-K
8 Performing a Measurement

8.4.2 Warning Messages absorption of air or water), and stability of the


measurement process. The operator’s awareness
and prevention of different sources of errors are
Automatic bubble detection essential to fully exploit the potential of the most
(FillingCheck™) accurate density meter on the market – the
DMA 5000 M.
If a bubble has been detected anywhere in the
U-tube in real time, the output field “Density Condi- The following tips may help to achieve highly accu-
tion” shows “Filling Warning” or “Error: No Oscilla- rate density results:
tion” for the current sample, and the message list
• Install the instrument in the right place.
quick access button changes: Instead of the green
OK mark, the yellow warning sign is displayed. See section 4.1 for the proper setup conditions.

TIP: For complete transparency and traceability of • High humidity or a measuring temperature
your sample filling and measurement process, below the ambient temperature may lead to
check the filling visually by means of the built-in condensation in the measuring cell.
camera (U-View™) in addition to the fully automatic To avoid condensation install a drying cartridge,
FillingCheck™. see section 8.8.
TIP: FillingCheck™ provides excellent support to • Be aware of the ambient pressure when you
the operator for samples of low and medium viscos- compare the measured result to a reference
ity ranges. value of a certified reference material.
The sensitivity of this feature depends on a combi- For example, the density of water between
nation of density, viscosity, and temperature, and is 970 mbar and 1013.25 mbar varies by approx.
not constant. For example, certain samples with 0.002 kg/m3.
high density (approx. 1.5 g/cm3) and medium vis- • Store samples and certified reference material
cosity (approx. 550 mPa·s) might generate a filling in a dark place at temperatures below 20 °C.
warning also for correctly filled samples. In all such Avoid temperature changes.
cases, changing the measuring temperature may
influence this combination so that FillingCheck™ • Installing the injection adapters 12 hours before
continues working as expected. the actual measurement or adjustment (e.g. the
day before) ensures relaxation of the measuring
Some samples may generate a filling warning even
cell as physical pressure or stress from the
when filled without bubbles, e.g. highly viscous
injection adapters has been applied during
samples or samples containing inhomogeneities.
installation.
In these cases we recommend to disable Filling-
Check™ and perform repeated measurements to • Setting the measuring temperature at least
validate the quality of filling. 12 hours before the actual measurement
(e.g. the day before) ensures temperature
stability of the whole measuring system.
Message list window
Mind that DMA M instruments operate in the
The appearance of the message list button in the mK range.
quick access area indicates the current error status
• The sample temperature should be slightly
(see section 5.1). Tapping the button opens the
higher than the measuring temperature. This
message list window showing the general status of
reduces the risk of degassing and the formation
the instrument and the measuring errors that have
of micro bubbles in the measuring cell.
occurred.
• Inconsistent results have been tracked down to
the use of plastic disposable syringes due to
8.5 Tips for Highly Accurate Density lubricants being dissolved by particular samples
or plastic being soluble in the liquid. For these
Measurements samples use glass syringes for filling.

In order to use the instrument’s full accuracy you • Set the precision class of the method used to
need to bring all measuring conditions close to their “Standard” (DMA 4100/4500 M) or “Precise”
ideal state. Sources of measurement uncertainty (DMA 5000 M) and activate the function
include environmental and measuring conditions, “Density stability criterion”.
sample handling, stability of the sample (e.g.

XDLIB016EN-K 31
8 Performing a Measurement

• Avoid influences of the syringe weight. nation of the sample. Sample containers must
Anton Paar provides a syringe holder, which is only be used once, right after opening the seal-
mounted on the density meter’s housing and ing.
comes already pre-installed on DMA 5000 M. • Volatile components of samples, like ethanol,
Follow the filling instructions in section 8.2. evaporate once the ampule or bottle is open
• Avoid residues of sample or cleaning agent in resulting in a change of density. The samples
the measuring cell due to insufficient drying have to be filled immediately after opening the
times. ampule or bottle. Close the measuring cell with
two male Luer plugs PTFE (mat. no. 63865) to
Depending on the nature of the sample, the
minimize the amount of vaporization of the filled
following characteristics may have a considerable
liquid (for DMA 4100/4500 M).
influence on the results of a density measurement:
• Ensure that your samples are completely homo-
• Be aware of the temperature dependence of geneous. Do not mix the samples by shaking
density. them vigorously, but by stirring them gently with
For example, samples like isooctane or dodec- a glass rod. Avoid any inclusions of micro-
ane have a thermal expansion coefficient close bubbles.
to 1 kg/(m3K) leading to a density change of
In conclusion, depending on the nature of the sam-
0.01 kg/m3 at a temperature change of only
ple, various error sources contribute to the mea-
10 mK (0.01 °C).
surement uncertainty. As an example, see fig. 15 for
• Hygroscopic samples, like ethanol, tend to the contributions to the measuring uncertainty of
absorb water from the air resulting in higher or isooctane.
lower density values compared to a stated refer-
ence value. The liquid samples have to be
injected immediately after opening the sealed
ampule or bottle. The longer the period between
opening and measuring the sample, the higher
the risk of a change of composition or contami-

Contributions to measurement uncertainty of isooctane


using a DMA 5000 M

6% 2%
Unce rtainty due to temperature
(temperature calibration)
12%
Unce rtainty of reference liquid

Specified repeatability of the


49% density measurement
12% Hand ling

Measuring temperature

Air p ressure
19%

Fig. 15: Contributions to uncertainty of isooctane

32 XDLIB016EN-K
8 Performing a Measurement

8.6 Degassing Samples 8.7 Special Filling Techniques


There are various methods to degas liquid samples.
Bubbling samples
The preferable method for your application depends
on the kind of sample and the amount of gas that is If the sample to be measured tends to form gas
dissolved in the sample. Pay attention to always bubbles, degas it before the measurement, see
treat all samples in the same way in order to get section 8.6.
reproducible measuring results.
If this is not possible, fill the sample at a temperature
IMPORTANT: Be aware of the fact that the compo- higher than the measuring temperature.
sition of some samples may slightly change during
the pretreatment due to the evaporation of volatile You can also put the instrument at a slight angle
components. (with spacers under the legs on the right of the
instrument), thus allowing the bubbles to escape
due to buoyancy.
Boiling the sample
Suspensions and emulsions
Suspensions or emulsions may tend to separate in
WARNING the measuring cell, giving incorrect results. Leave
Samples containing toxic volatile compounds such samples in the measuring cell as briefly as
can cause irritation and serious injuries to your possible. Preheat or precool them before filling.
eyes, skin and mucous membranes, as well as It may help to put spacers under the legs on the left
toxication. of the instrument, thus putting it at an angle to coun-
• If your sample contains volatile compounds that terbalance the separation force generated by the
are toxic, always handle it in an appropriate oscillation of the measuring cell.
environment, like under a fume hood, espe-
cially when you boil your sample.
Highly viscous samples
Highly viscous samples can be heated up to lower
the viscosity. Always heat the sample to a tempera-
WARNING ture that is approx. 15 °C (27 °F) higher than the
measuring temperature, which can be 100 °C maxi-
When you boil flammable liquids, there is a risk mum.
of fire. Serious injuries are possible.
• Do not boil flammable liquids. Pastes
1. Boil the liquid for several minutes to remove Paste-like materials like toothpaste or tomato
dissolved air. ketchup can be filled by syringe. Inject these kinds
of samples into the measuring cell by pushing the
2. Fill the boiled liquid into a clean glass flask and plunger very slowly and steadily.
cover it.
If the samples have a very high viscosity, you can fill
3. Wait until the liquid has cooled down approxi-
them into the syringe by pulling the plunger com-
mately to measuring temperature.
pletely out of the syringe, filling the sample from the
back using a spoon, and then remounting the
Stirring the sample plunger.
• Stir your sample vigorously for 2–15 minutes
(depending on the stirring equipment) until Liquids in aerosol cans
bubbling ceases.
For the quality control of aerosol cans, you can use
• You can pour the sample through a paper filter the Anton Paar Aerosol Adapter (mat. no. 74650) to
after stirring to degas it even more efficiently. fill the liquid safely and conveniently into your
DMA M. For details see the manual of the Aerosol
Using an ultrasonic bath Adapter.

• Put your sample for approx. 5–10 minutes into


an ultrasonic bath until bubbling ceases.

XDLIB016EN-K 33
8 Performing a Measurement

Gases For a measuring temperature of 20 °C, a drying


cartridge must be used under the following condi-
It is possible to measure gases with a DMA M. For tions:
details contact your local Anton Paar representative
and ask for the corresponding application report and ambient temperature relative air humidity
the necessary accessories.
20 °C > 70 %
25 °C > 50 %
8.8 Measuring at Low Temperatures / 30 °C > 38 %
under High Humidity Conditions
To regenerate moist silica gel
If the ambient air is humid, and the measuring tem-
perature is lower than the ambient temperature, The drying cartridge contains silica gel, a non-toxic
condensation may occur in the measuring cell and drying agent. When active, the color of the drying
the measuring cell block. agent is orange. Silica gel having absorbed liquid
turns green.
Condensation in the measuring cell causes adjust-
ment and measurement errors. Condensation in the Moist silica gel can be regenerated:
measuring cell block damages the electronics and • Pour the silica gel into a glass bowl and blow
may lead to a failure of the U-view™ function. The hot, dry air (max. 130 °C / 266 °F) through it for
higher the difference between the set measuring approx. 5 hours, or place it in a laboratory oven
temperature and ambient temperature, and the for a few hours (or overnight) until its color is
higher the air humidity, the easier condensation orange again.
occurs.
NOTICE
8.8.1 Preventing Condensation in the Do not use higher drying temperatures than
130 °C (266 °F). Otherwise the indicator function
Measuring Cell of the silica gel will be spoiled.

To prevent condensation in the measuring cell, use


a drying cartridge (mat. no. 65085) and connect it to 8.8.2 Removing Condensation From the
the “DRY AIR IN AIR PUMP” connector at the rear
of the instrument, see fig. 16. Camera
1. Cut a piece of approx. 75 cm (29.5 in) length
NOTICE from the silicone hose included in the accessory
• Never connect hoses containing liquids or kit.
moist gases to the “DRY AIR IN AIR PUMP”
2. Connect one end of the silicone hose to the air
connector as this may lead to condensation in
pump outlet on the right of the instrument.
the measuring cell and subsequently to mea-
surement and adjustment errors. 3. Connect the other end of the silicone hose to
• Operate the “DRY AIR IN AIR PUMP” connec- the “DRY AIR IN BLOCK” connector at the rear
tor only at ambient pressure. of the instrument.
4. Set the measuring temperature of the instru-
ment to 100 °C.
5. Start the air pump after the temperature has
been reached.
6. Turn off the air pump after approx. 15 minutes.

DRY AIR IN
AIR PUMP

DRY AIR IN
BLOCK

drying cartridge

Fig. 16: Drying cartridge connected

34 XDLIB016EN-K
8 Performing a Measurement

8.8.3 Preventing Condensation in the • Degas your samples thoroughly directly before
measuring, see section 8.6.
Measuring Cell Block
• Heat your samples up to a temperature signifi-
To prevent condensation in the measuring cell cantly higher than the measuring temperature
block, connect a dry air supply to the “DRY AIR IN with stirring, directly before measuring.
BLOCK” connector at the rear of the instrument
using a 3x5 mm hose made of suitable material To measure highly viscous samples at high
(e.g. silicone) (see fig. 16). temperatures
See section 8.7.
NOTICE
Never connect hoses containing liquids or moist
gases to the “DRY AIR IN BLOCK” connector as
this may lead to damage of the electronics.
8.10 Measuring at High Pressures
The supplied silicone hose and injection adapters
The dry air supply must be used additionally to the can only be used at atmospheric pressure. Before
drying cartridge if the measuring temperature is you apply high pressures, exchange the supplied
more than 5 °C lower than the ambient temperature. filling components with pressure-resistant compo-
The following specifications of the applied air are nents.
required:
- 0.03 bar (0.435 psi) rel.
- max. volumetric flow rate: 80 L/h WARNING
- class 5 according to ISO 8573-1
- max. particle size: 40 µm Leaky components of the measuring system can
- max. pressure dew point: 10 °C below cause sample to splash out when pressure is
measuring temperature applied to the measuring system. Injuries and
- max. oil content: 25 mg/m3 risk of fire possible.
To avoid injuries, do the following:
• At pressures higher than ambient pressure,
8.9 Measuring at High Temperatures only use the injection adapters DMA/CarboQC
(mat. no. 159537) and polyurethane hoses
2x4 mm (mat. no. 135259).
• Do not exceed the maximum operating
WARNING pressure of any single component.
• Before you start a measurement at high
Risk of leakage pressure, check the pressure tightness of the
At high sample temperatures in combination with system with air.
high pressure the injection adapter Luer may leak. • If you measure any aggressive, poisonous, or
• At measuring temperatures of 50 °C (122 °F) flammable sample at high pressure, use only
and higher, the applied pressure must be the smallest possible sample amount.
limited to 5 bar (72.5 psi) absolute pressure.

Adjustment with air and water


To prevent bubble formation
To reach the highest possible accuracy for high
If you measure samples at temperatures significantly pressure measurements, perform the air adjustment
higher than ambient temperature, the tendency to as usual at ambient pressure, and the water adjust-
form gas bubbles in the measuring cell will dramati- ment or an adjustment with any other reference
cally increase. To ensure precise results, you can: liquid at the pressure at which you are going to
perform the measurements.

XDLIB016EN-K 35
9 Checks, Adjustments, Calibrations

9 Checks, Adjustments, Calibrations


9.1 Definitions Custom checks are defined for a certain method and
are always performed at the temperature of the
selected method with the corresponding precision
Check class.
Checking the correct operation of an instrument by Air checks and water checks are available for any
measuring a sample of exactly known measurement method.
properties, and comparing the results with the
If the instrument is operated in the non-storage
expected values.
mode, no check data will be stored, see also the
General Software Functions Manual, section 9.1.2.
Adjustment
IMPORTANT: When operating the instrument in the
Ensuring correct measurements in the future by non-storage mode, print or export the check results
filling a sample of exactly known measurement immediately after the check. Otherwise the check
properties (standard) and adjusting the instrument data will be lost.
constants in a way that the known correct results are
delivered by the instrument. When to do water checks and custom
For a successful adjustment, usually at least two checks
standards are needed with measurement properties
that encompass the expected measurement results Use the water check and a custom check to verify
of your samples. that the instrument is measuring with satisfactory
accuracy. We recommend to perform a water check
or a custom check every day before you start your
Calibration measurements.
Calibrations are check procedures that are carried Perform additional water checks or custom checks
out using certified standards. By comparing the as required and at your own discretion, e.g. when
measured result with the standard reference value, you get unexpected results.
you can validate the quality of your measurements.
When to do air checks
9.2 Checks Use the air check to verify the efficiency of your
cleaning and drying procedure. We recommend to
By checks, carried out in regular intervals, you can perform an air check every day after the measure-
ensure that your density and concentration mea- ments have been finished and the measuring cell
surements consistently deliver results of high and has been cleaned and dried.
stable accuracy.
Perform additional air checks as required and at
With a density check, you fill a medium of known your own discretion, e.g. after the measurement of
density (air, water, or any standard liquid specific to critical samples that might stick to the measuring
your needs) into the measuring cell and compare cell (e.g. samples containing adhesives, sticky
the measured density with the reference value. particles, proteins).
DMA 4100/4500/5000 M perform the water checks
and air checks automatically at the measuring tem- 9.2.1 Check Settings
perature of the currently active method. The preci-
sion class used for the check is also according to the You can edit the name, method (custom check only),
currently active method. The densities of water and time interval, and the tolerance of density checks.
air at the measuring temperature are calculated and
compared with the actually measured values. With
water checks and custom checks, the values are
Tolerances
calculated for the set temperature. With air checks, The factory presets for both air checks and water
the value is calculated for the set temperature and checks are:
the measured air pressure.

36 XDLIB016EN-K
9 Checks, Adjustments, Calibrations

- Use the check box “Check execution remind-


DMA M model Tolerance er” to define whether the check is obligatory,
DMA 4100 M 0.0002 g/cm3 and enter a time interval in days.
- Use the check box “Prohibit measurements
DMA 4500 M 0.0001 g/cm3
after expiry” to define whether checks are
DMA 5000 M 0.00005 g/cm3 obligatory for subsequent measurements.
IMPORTANT: If measurements after the expiration
Editing the settings of the air check and the of a check are prohibited, you cannot start the check
water check via the quick settings.
1. Tap <Menu> and select Setup > Expert Settings 5. Tap <Next> and perform the following settings:
> Check Management to open the check admin- - Select a quantity and the corresponding unit.
istration list. - Define the check tolerance by the “Lower
2. Highlight “AirCheck” or “WaterCheck”, respec- limit” and “Upper limit”.
tively, and tap <Edit> to open the “Check Admin- - Optionally define the settings for further
istration” wizard. quantities in the same way.
3. Enter a name for the check and tap <Next>. 6. Tap <OK>.
4. Perform the following settings:
- Use the check box “GxP relevant” to define Editing the settings of a custom check
whether the check is relevant for “Good 1. Tap <Menu> and select Setup > Expert Settings
Practice” quality guidelines and regulations. > Check Management to open the check admin-
- Use the check box “Check execution remind- istration list.
er” to define whether the check is obligatory,
2. Highlight a custom check and tap <Edit> to
and enter a time interval in days.
open the “Check Administration” wizard.
- Use the check box “Prohibit measurements
after expiry” to define whether checks are 3. Change the settings as required.
obligatory for subsequent measurements.
IMPORTANT: If measurements after the expiration 9.2.2 Performing a Check
of a check are prohibited, you cannot start the check
via the quick settings. 1. Tap <Menu> and select Checks/Adjustments >
Checks to open the checks list.
5. Tap <Next>.
2. Highlight a water check, an air check, or a
6. Define the maximum allowed “Lower deviation”
custom check in the list.
and “Upper deviation”.
3. Tap <Start> and follow the instructions on the
7. Tap <OK>.
screen.
- For a water check, use freshly degassed
Defining a custom check
ultra-pure water.
1. Tap <Menu> and select Setup > Expert Settings - For an air check, clean and dry the measur-
> Check Management to open the check admin- ing cell thoroughly.
istration list. - Use the camera image to check that the
measuring cell is clean or that water has
2. Tap <New> to open the “Check Administration”
been filled free from bubbles.
wizard.
When the check is finished, the following infor-
3. Perform the following settings:
mation is displayed:
- Enter a name for the check.
- Check name/type and check result
- Select the method to define detailed method
(“Passed” or “Not passed”)
settings for the check.
- Date and time
4. Tap <Next> and perform the following settings: - Method used
- Use the check box “GxP relevant” to define - Check result
whether the check is relevant for “Good - User name
Practice” quality guidelines and regulations.

XDLIB016EN-K 37
9 Checks, Adjustments, Calibrations

- For water checks: IMPORTANT:


- Reference value calculated for the set • Auto air check results will not be saved in the
temperature check data memory.
- Lower deviation • Auto air check limits are set according to the air
- Upper deviation check limits.
- Measured value
- Check result Auto air check procedure
- Set temperature for the density cell
- For air checks: If a measurement is started, and the auto air check
- Reference value calculated for the set function is activated, the instrument will initiate an
temperature auto air check automatically.
- Lower deviation
1. Check that the density measuring cell is clean
- Upper deviation
(you can also use the camera image). Clean
- Measured value
and dry the measuring cell thoroughly if
- Check result
necessary.
- Air pressure
- Set temperature for the density cell 2. Tap <OK> to start the auto air check procedure.
- For custom checks: - If the auto air check succeeds, fill the sample
- Lower limit into the measuring cell and start your mea-
- Upper limit surement by tapping <OK>.
- Measured value - If the auto air check fails, you can take correc-
- Check result tive actions and restart the auto air check by
- Set temperature for the density cell tapping <OK>, or you can cancel the
4. Tap <Print or Export> if you want to print or measurement by tapping <Cancel>.
export the results of the check.
5. Tap <OK> or <Home> to exit the check routine. 9.2.4 Viewing, Printing, or Exporting
Current Check Data
If the water check has failed
Not available in non-storage mode.
We recommend taking corrective actions until the
check is valid again: The total number of entries in the check history is
limited to 110.
• Examine the camera image included in the
results to check that the water has been filled
bubble-free (see section 8.2). To view check data
• Check the quality of the water. 1. Tap <Menu> and select Data Memory > Check
• Clean the measuring cell thoroughly. Data.
• If above actions do not help, perform an An overview of the available check data is
air/water adjustment. displayed.
2. To view check data in detail, highlight a list item
and tap <Details>.
9.2.3 Auto Air Check
To print or export check data
Activating/deactivating the auto air check
1. Tap <Menu> and select Data Memory > Check
An auto air check can be initiated automatically Data.
before each measurement to verify that the measur-
2. To print all check data on paper or to a PDF file,
ing cell is clean.
or to export all check data as an MS Excel file
1. Tap <Menu> and select Setup > Measuring or text file, tap <Print or Export> and follow the
System Settings > Density Module. instructions on the screen.
2. Use the check box to activate/deactivate the 3. To print or export single check data, tap
auto air check function. <Details> and then <Print or Export>.
3. Tap <OK>. Use and to scroll through the data list.

38 XDLIB016EN-K
9 Checks, Adjustments, Calibrations

9.3 Adjustments The factory adjustment has been set using refer-
ence values for the density of air (humidity 50 %)
and water based on the formula of Spieweck and
If the instrument is operated in the non-storage
Bettin1,3. This formula covers the whole measuring
mode, the adjustment data are not viewable, see
also the General Software Functions Manual, range (0–100 °C) of the instrument.
section 9.1.2. IMPORTANT: You have to readjust the instrument
IMPORTANT: When operating the instrument in the after changing the selected air and/or water table.
non-storage mode, print or export the adjustment 1. Tap <Menu> and select Setup > Measuring
results immediately after the adjustment. System Settings > Density Module.
2. Use the drop-down box “Air Table” to select the
9.3.1 Air/Water Adjustment preferred reference table.
3. Use the drop-down box “Water Table” to select
An air/water adjustment has to be performed if the the preferred reference table.
water check has failed (“not passed” as the result),
4. Tap <OK> to save your settings.
and using freshly degassed ultra-pure water and
cleaning the measuring cell did not help. TIP: For use in metrology, the CIPM density formula
is the preferred standard over its recommended
The adjustment media are dry air and freshly
range (0–40 °C) at pressures near atmospheric.
degassed ultra-pure water.
The formula should not be extrapolated outside this
The ThermoBalance™ technology allows for pre- range.
cise measurements over the whole temperature Densities from the IAPWS formula are consistent
range with only one adjustment at 20 °C. To achieve with the CIPM standard within the range of validity
the highest possible precision of measurements at of the CIPM formula. Outside the CIPM range of
different temperatures, you can additionally perform validity, the IAPWS formula is the preferred method
a temperature range adjustment, see section 9.3.2. for obtaining accurate densities of water.
The air/water adjustment takes 5–10 minutes if the IMPORTANT: The choice of reference table also
instrument is already clean and dry and equilibrated affects derived quantities (e.g. Apparent Density,
to 20 °C. SG, API values, etc.).
All factory-set concentration tables consist of
The adjustment procedure can be aborted by
calculated data based on the reference values
tapping <Cancel>.
according to Spieweck and Bettin.

To set the reference values for the To perform an air/water adjustment


air/water adjustment
1. Tap <Menu> and select Checks/Adjustments >
The reference values for air can be selected accord- Air/Water at 20 °C.
ing to your needs. They are either based on the
formula of 2. Rinse and dry the measuring cell.

- Spieweck and Bettin1 or TIP: If you use undenatured ethanol as the final
- CIPM2. rinsing liquid, only 3–4 minutes drying time are
required.
The reference values for water can be selected
according to your needs. They are either based on Tap <Air Pump on> to dry the measuring cell.
the formula of 3. Tap <OK>.
- Spieweck and Bettin3 or 4. Enter the air humidity and the atmospheric
- CIPM4 / IAPWS5. pressure.
(The CIPM formula is limited to 0–40 °C only, The air humidity is set to 50 % per default.
so for temperatures above 40 °C, the IAPWS
The atmospheric pressure displayed is
formula is used.)
measured automatically by a built-in sensor.
1 F. Spieweck, H. Bettin: Review: Solid and liquid density determination. tm – Technisches Messen 59 (1992) 7–8, pp. 285–292.
2 A. Picard, R.S. Davis, M. Gläser, K. Fujii. Metrologia 45 (2008), pp. 149–155.
3 Cf. Spieweck/Bettin, p. 291.
4 M. Tanaka, G. Girard, R. Davis, A. Peuto, N. Bignell. Metrologia 38 (2001), pp. 301–309.
5 International Association for the properties of water and Steam: Release on the IAPWS formulation 1995 for the
thermodynamic properties of ordinary water substance for general and scientific use [1996]. Available at www.iapws.org.

XDLIB016EN-K 39
9 Checks, Adjustments, Calibrations

5. Tap <OK>. The adjustment procedure can be aborted by tap-


The air adjustment routine is carried out. ping <Cancel>.

6. Fill freshly degassed ultra-pure water into the 1. Tap <Menu> and select Checks/Adjustments >
measuring cell and tap <OK>. Other Adjustments > Density Module >
Air/Water Wide Range.
Be careful to fill the water without air bubbles.
2. Follow the instructions on the screen.
TIP: If the water has been filled without air bubbles,
you can ignore a possible warning message Check that the water is filled without air bubbles.
“Density Condition: filling warning” during the TIP: If the water has been filled without air bubbles,
adjustment routine. A proper adjustment is required you can ignore a possible warning message
for the FillingCheck™ function. “Density Condition: filling warning” during the
The water adjustment routine is carried out. adjustment routine. A proper adjustment is required
for the FillingCheck™ function.
When the adjustment is finished, the following
information is displayed:
- Reference density of water 9.3.3 Adjustment of the Built-in
- Deviation to reference value using old Atmospheric Pressure Sensor
adjustment constants
- Deviation to reference value using new 1. Tap <Menu> and select Checks/Adjustments >
adjustment constants Other Adjustments > DCB Module >
7. Check the recommendation on the screen and Atmospheric Pressure Sensor Adjustment.
select one of the options <Reject>, <Print>, or 2. Use a calibrated external pressure sensor to
<Apply>. determine an exact value for the atmospheric
pressure.
9.3.2 Air/Water Wide-Range Adjustment IMPORTANT: Do not use the atmospheric pressure
that you can get from a local weather station because
IMPORTANT: An air/water wide-range adjustment it is usually not the absolute atmospheric pressure,
can only be performed if the air table of Spieweck/ but a calculated atmospheric pressure value refer-
Bettin is set as reference table, see section 9.3.1. enced to sea level.
Perform an air/water wide-range adjustment before 3. Enter the atmospheric pressure (in hPa) and
the air/water density adjustment to achieve the tap <OK>.
maximum accuracy for measurements at different 4. Enter the barometer ID and tap <OK>.
temperatures.
5. Tap <OK> to start the adjustment.
The air/water wide-range adjustment performs a Wait for the adjustment to finish.
sequence of water adjustments followed by air
adjustments at the temperatures listed in table 7. 6. Check the recommendation on the screen and
select one of the options <Reject>, <Print>, or
Table 7: Air/water wide-range adjustment – <Apply>.
sequence of adjustments and temperatures
The final value may deviate from the one that
Water adjustments Air adjustments you have entered by up to ±7 hPa. This will not
influence the measuring accuracy.
1 60 °C (140 °F) 4 20 °C (68 °F)
2 40 °C (104 °F) 5 40 °C (104 °F)
9.3.4 Performing Special Adjustments
3 20 °C (68 °F) 6 60 °C (140 °F)
7 80 °C (176 °F) Not available in non-storage mode.
8 100 °C (212 °F)
Duration: approx. 90 minutes 9.3.4.1 Special Adjustments
Special adjustments are user-specific adjustments
The adjustment media are dry air and freshly for special density units, concentrations and tem-
degassed ultra-pure water. peratures. After a successful adjustment procedure,
To ensure bubble-free filling, preheat the water to
approx. 60 °C.

40 XDLIB016EN-K
9 Checks, Adjustments, Calibrations

the special adjustment can be used as a standard - Use the drop-down box “Adjustments” to
measuring quantity that is displayed and printed. It select one of the 5 available special adjust-
can also be used: ment slot positions.
- Enter name and unit for the special adjust-
- as an input parameter for a user function
ment.
- as the API input quantity
- Set the temperature for the adjustment.
- as the input quantity for the Canadian excise
alcohol table 3. Tap <Next>.

Five different special adjustments can be stored. For 4. Enter the reference values for the first and
each special adjustment name, unit, and tempera- second reference medium.
ture can be specified. 5. Tap <Next>.
During a special adjustment, adjustment coefficients The special adjustment routine starts.
are calculated from the oscillation periods of two 6. Rinse and dry the measuring cell.
reference media with known density according to
Tap <Air Pump on> to dry the measuring cell.
the following formula:
7. Fill the first reference medium into the
2 measuring cell and tap <OK>.
 = A  PQ – B
Check that the medium is filled without air
ρ ....... reference density of medium bubbles.
A, B .. adjustment coefficients 8. Rinse and dry the measuring cell.
PQ .... oscillation period of medium
Tap <Air Pump on> to dry the measuring cell.
Hints for measurements using special 9. Fill the second reference medium into the
measuring cell and tap <OK>.
adjustments
Check that the medium is filled without air
• If you measure using a special adjustment, the bubbles.
set measuring temperature must be the same
10. Check the recommendation on the screen and
as the temperature at which the special adjust-
select one of the options <Print>, <Reject>, or
ment has been performed. Otherwise no results
<Apply>.
can be obtained.
After successful adjustment, the determined
• No viscosity correction is available if the instru-
special adjustment coefficients are stored. A
ment is operated using a special adjustment.
new output quantity is generated in the group
• No adjustment history is available for special “Special Adjustments”, which is calculated
adjustments. using these coefficients.
• Special adjustments can be performed at any TIP: The new output quantity will only calculate valid
set temperature within the measuring tempera- results in methods using the same set temperature
ture range of your instrument. as the special adjustment, on which the quantity is
based.
Prerequisites for the reference media
The densities of the two reference media used for a 9.3.4.2 Special Adjustment for the Canadian
special adjustment have to differ by at least Excise Alcohol Table
Δ ρ = 0.01 g/cm3.
To use the output quantity “Canadian Excise Alcohol
The PQ-values of the adjustment media have to Table” (see appendix B), it is necessary to perform
differ by at least 0.0001. a special adjustment with apparent density values of
air and water, and link that adjustment to the Cana-
To perform a special adjustment dian Excise Alcohol Table.
1. Tap <Menu> and select Checks/Adjustments > 1. Perform a special adjustment with air and water
Other Adjustments > Density Module > Special using apparent density for the reference values.
Adjustments. 2. Link the special adjustment to the Canadian
2. Perform the following settings: Excise Alcohol Table.
3. Select the table for output fields, result outputs
and the data browser.

XDLIB016EN-K 41
9 Checks, Adjustments, Calibrations

9.3.5 Viewing, Printing, or Exporting • Tap <Menu> and select Data Memory > Adjust-
ment Data > Density Module > Density Adjust-
Adjustment Data ment Trend.
Not available in non-storage mode. - Tap on the graph to activate the zoom
function.
You can view, print, and export the detailed data for - Use the magnifiers below the graph to
the last 50 adjustments, both for density and zoom in and out.
temperature. - Use the arrows to move from one data
TIP: Inconsistent adjustment data can be the result point to the previous or next one.
of changing the reference tables for air and water, - Use the data point bar to scroll within the
see section 9.3.1. graph.
- To close the zoom function, tap <X> in the
upper right corner.
To view adjustment data - To print out the graph on paper or to a PDF
1. Tap <Menu> and select Data Memory > Adjust- file, tap <Print or Export> and follow the
ment Data > Density Module, then select instructions on the screen.
“Density Adjustment”, “Special Adjustment” or RS-232 printers with paper roll cannot print
“Temperature Adjustment” to open the corre- the adjustment trend graph.
sponding adjustment list.
2. To view the adjustment data in detail, highlight a 9.3.7 Resetting the Adjustment Data to
list item and tap <Details>.
Factory Adjustment
To print or export single adjustment data You can re-activate the factory adjustment for the
density measurement.
1. Tap <Menu> and select Data Memory > Adjust-
ment Data > Density Module, then select 1. Tap <Menu> and select Checks/Adjustments >
“Density Adjustment”, “Special Adjustment” or Other Adjustments > Density Module > Reset
“Temperature Adjustment” to open the corre- To Factory Adjustment.
sponding adjustment list.
2. Activate the check box “Density Module” and
2. To print or export single adjustment data, high- tap <OK>.
light a list item, tap <Details> and then <Print or The instrument will restart.
Export>.
IMPORTANT: Factory default reference values for
Use and to scroll through the data list.
the density of air and water are based on the formula
of Spieweck and Bettin, see section 9.3.1.
To print or export all adjustment data
1. Tap <Menu> and select Data Memory > Adjust- 9.3.8 Adjustment Analysis
ment Data > Print or Export Adjustment Data.
2. To print out all adjustment data on paper or to a Not available in non-storage mode.
PDF file, or to export all adjustment data as an
The adjustment analysis function is based on an
MS Excel or text file, activate the check box
evaluation of the instrument constants, which are
“Density Module”, and tap <OK>.
determined during an adjustment. If the adjustment
analysis is activated, the instrument will automati-
9.3.6 Viewing, Printing, or Exporting cally compare the latest adjusted constants to those
of the reference adjustment. If the adjustment sig-
Adjustment History: Adjustment Trend nificantly deviates from the reference adjustment,
the instrument will generate a warning. Therefore, it
Not available in non-storage mode. is important to perform the adjustment procedure
You can view the values of constant B (see properly.
section 2.1) for the last 50 adjustments as a graph. A deviation may be caused by an improper adjust-
You can print or export the adjustment trend graph ment (e.g. insufficient drying before air adjustment,
together with a list of the values of constant B. presence of gas bubbles or impurities), removal of
cell material due to aggressive liquids, or due to
built-up deposits in the measuring cell.

42 XDLIB016EN-K
9 Checks, Adjustments, Calibrations

TIP: Fluctuations are most probably caused by


variations in the air density due to varying weather NOTICE
conditions. Such fluctuations can be avoided by • Always check the expiry date of the calibration
entering the current barometric pressure before the liquids.
air adjustment. • Store the calibration liquids in a cool and dark
place.
TIP: Inconsistent adjustment data can be the result • Use the calibration liquids immediately and
of changing the reference tables for air and water, only once after the container has been opened.
see section 9.3.1.
TIP: Take a look at the adjustment trend graph to To perform a calibration
obtain additional information on the quality of your
adjustments. While deposits inside the U-tube are 1. Perform a water check.
indicated by increasing values, cell removal is 2. If necessary, perform an air/water adjustment at
indicated by decreasing values. 20 °C.
3. Thoroughly clean and dry the measuring cell.
To activate / deactivate adjustment analysis
4. Select a measuring method with the following
1. Tap <Menu> and select Setup > Measuring settings:
System Settings > Density Module.
- set temperature equals the temperature of
2. Activate or deactivate the adjustment analysis the certified reference value
functionality. - precision class “Precise”
3. Tap <Set Reference Adjustment> and <OK> to - check density stability: enabled
set the current adjustment as the new reference 5. Open the bottle with the liquid density standard.
adjustment.
TIP: If your bottle with density standard has a sep-
tum, we recommend that you pierce it carefully with
9.4 Calibration any clean, sharp tool, then fill a Luer tip syringe with
standard liquid by pushing the tip into the hole of the
septum, holding the bottle upside down, and slowly
The goal of a calibration is to validate the accuracy
pulling the plunger.
of the density measurement.
See also section 8.5 for recommendations.
To calibrate the instrument, measure a certified
6. Immediately after opening the bottle inject the
standard liquid and compare the result to the refer-
standard into the measuring cell.
ence value indicated in the calibration certificate of
the standard. 7. Perform a measurement.
The physical properties (density, viscosity) of the TIP: If you have enough standard liquid, we recom-
liquid density standards should be similar to those of mend to do a series of three measurements and
the samples. take the arithmetic average of the results.
The frequency of calibrations with certified liquid 8. After the measurement is finished, print the
density standards depends on your requirements result.
and judgment. Recommendation: 1–2 calibrations 9. Document the calibration procedure in a calibra-
per year. tion record containing the operator's name, the
date, place, description and results of the cali-
bration procedure, and the calibration certificate
of the liquid density standard.

XDLIB016EN-K 43
10 Upkeep and Cleaning

10 Upkeep and Cleaning


To ensure a constant and high accuracy of your Recommended for aqueous samples / beverages:
measurements, employ a regular and effective water (cleaning liquid 1) and non-denatured ethanol
cleaning routine, and store the instrument under the (cleaning liquid 2).
recommended conditions.
Recommended for petrochemical samples:
petroleum naphtha (cleaning liquid 1) and acetone
10.1 Cleaning and Drying the (cleaning liquid 2).

Measuring Cell Further recommendations can be found in


appendix E.
If you are not sure whether a cleaning liquid is suit-
able for your sample, perform a preliminary test in a
WARNING
test tube to see if any phase separation, precipitate
Risk of injuries and fire by liquids leaking or opalescence can be observed.
Before you fill any sample or cleaning liquid into
the instrument: Cleaning and drying procedure without
• Strictly follow all safety instructions concerning Xsample filling equipment
the use of chemicals and the use of flammable
chemicals, see section 1; 1. Rinse the measuring cell with cleaning liquid 1
• Make sure that all wetted parts are resistant, (minimum 5 mL).
see appendix A.3. If your sample is viscous or contains particles,
use more cleaning liquid.
NOTICE 2. Empty the measuring cell.
Do not use any mechanical action for cleaning 3. Rinse the measuring cell with cleaning liquid 2
the measuring cell. (minimum 5 mL).
4. Empty the measuring cell.
Cleaning frequency
Clean and dry the measuring cell at least after each
working day or working shift.
Cleaning more frequently can be necessary ...
- before you perform adjustments,
- before you want to measure using a minimum
sample amount,
- before you measure a sample that is not
miscible with the previous sample
(e.g. water after a petrochemical sample),
- before you measure a sample that could
chemically react with the previous sample.

Cleaning liquids
For cleaning and drying, employ two cleaning liquids
in a row:
• Cleaning liquid 1 dissolves and removes sample
residues in the measuring cell. It has to be a
good solvent for all sample components.
• Cleaning liquid 2 removes cleaning liquid 1 and
is easily evaporated by a stream of dry air so
that drying of the cell is accelerated. Cleaning Fig. 17: Drying the measuring cell
liquid 2 has to be a good solvent for cleaning
liquid 1.

44 XDLIB016EN-K
10 Upkeep and Cleaning

5. Insert the air pump hose with the adapter Luer


cone into the sample inlet adapter or into the
top connector of the syringe holder, see fig. 17. WARNING
6. Tap in the quick access area to start the air
Ethanol is a highly flammable liquid.
pump.
• Strictly follow all safety instructions concerning
7. Wait until the measuring cell is dry (stable the use of flammable chemicals, see section 1.
density reading).
The time needed depends on the vapor pres-
sure of cleaning liquid 2 and the temperature of
NOTICE
the measuring cell (ethanol at 20 °C: approx. Corrosion due to unsuited means of cleaning
5 min, acetone at 20 °C: approx. 3 min). Using substances for cleaning that are not suit-
able causes corrosion of the instrument housing.
If the ambient humidity is > 90 % rel. humidity, Never use:
use a drying cartridge (see section 8.8) to • highly nonpolar solvents (e.g. toluene, hexane,
reduce the drying time. solvent naphtha),
8. Tap in the quick access area to stop the air • strong acids or bases (e.g. nitric acid, sulfuric
pump, or wait for the pump timeout. acid, hydrochloric acid, caustic soda),
9. Disconnect the air pump hose with the adapter • strong mechanical action (steel brush).
Luer cone.
To clean the instrument housing or the touchscreen,
use a soft tissue, which can be wetted with ethanol
or warm water, if necessary with some mild cleaning
WARNING agent added (pH < 10).
Risk of injuries and fire by liquids leaking
If liquids get into the air pump system, they may
destroy the pump diaphragm and leak from the 10.3 Storing the Instrument
instrument.
• Disconnect the air pump hose before you start Clean and dry the measuring cell, see section 10.1,
filling liquids. before you store the instrument for more than one
day. Otherwise algae may grow on the glass sur-
face, which are difficult to remove.
Cleaning and drying procedure with
If you store the instrument for less than one day, the
Xsample filling equipment measuring cell can be filled with ultra-pure water or
See the manual of the Xsample. stay filled with the last cleaning liquid used. If you
have filled by syringe, leave the syringe connected
to the injection adapter to prevent spillage of the
10.2 Cleaning the Instrument Housing liquid.

and the Touchscreen


10.4 Transporting the Instrument
WARNING • Empty the measuring cell and all hoses before
you move or lift the instrument.
Before using any cleaning agents for the instru- • To move or lift the instrument, grasp the ledge
ment’s housing and touchscreen: on top of the instrument at the back with one
• Strictly follow all safety instructions concerning hand. Place the other hand under the display at
the use of chemicals and the use of flammable the front. There is a hollow for your fingers.
chemicals, see section 1.
• Carry the instrument in front of you and keep it
• Make sure that all parts of the housing are
close to your body.
resistant, see appendix A.2. In case of
uncertainties contact Anton Paar GmbH.
• Decontaminate and remove aggressive sample
residues on the instrument.

XDLIB016EN-K 45
11 Maintenance and Repair

11 Maintenance and Repair


11.1 Maintenance Performed by an • cables
• fuses
Authorized Anton Paar Service • batteries
• desiccants
Engineer • protection foils and covers
The instrument requires a periodical maintenance, All parts damaged in consequence of a fall of the
which shall be performed by an authorized instrument are generally excluded from the warranty
Anton Paar Service Engineer. 1 as well.
A missing maintenance may mean that under
certain conditions your warranty is no longer valid. 2 11.2 Repair Performed by an Autho-
Maintenance interval rized Anton Paar Representative
once a year In case your instrument needs repair, contact your
local Anton Paar representative, who will take care
Parts to be exchanged at every mainte- of the necessary steps. If your instrument needs to
nance interval (wear and tear parts) be returned, request an RMA (Return Material
Authorization Number). It must not be sent without
• hoses the RMA and the filled “Safety Declaration for Instru-
• adapters ment Repairs”. Please make sure it is cleaned
before return.
Following parts are generally excluded TIP: Contact your local Anton Paar representative
from the warranty (wear and tear parts) from the Anton Paar website under “Contact”
(https://www.anton-paar.com).
• syringes
• hoses IMPORTANT: You must not return instruments that
• adapters, connectors, fittings are contaminated by radioactive materials, infec-
• pump diaphragms tious agents, or other harmful substances that cause
• filters health hazards.
• O-rings, seals, gaskets

1 Please contact your Anton Paar representative to get an offer.


2 For detailed information see the general terms of delivery (GTD) on the Anton Paar website (https://www.anton-paar.com).

46 XDLIB016EN-K
Appendix A: Technical Data

Appendix A: Technical Data


A.1: Specifications
Table 8: Measuring performance

DMA 4100 M DMA 4500 M DMA 5000 M


Density
Measuring range 0 g/cm3 to 3 g/cm3
Repeatability s.d.a 0.00001 g/cm3 0.000005 g/cm3 0.000001 g/cm3
Reproducibility s.d.a 0.00005 g/cm3 0.00002 g/cm3 0.000005 g/cm3
Accuracyb 0.0001 g/cm3 0.00005 g/cm3 0.000007 g/cm3
(full range)
0.00001 g/cm3
(0–1 g/cm3, 15–20 °C)
Temperature
Measuring rangec 0 °C to 100 °C (32 °F to 212 °F)
Repeatability s.d. 0.02 °C (0.04 °F) 0.01 °C (0.02 °F) 0.001 °C (0.002 °F)
Accuracy 0.03 °C (0.05 °F) 0.02 °C (0.04 °F) 0.01 °C (0.02 °F)
(full range)
0.01 °C (0.02 °F)
(15–20 °C)

Pressure ranged up to 10 bar (145 psi) absolute pressure


e
Measuring time approx. 30 s approx. 30 s approx. 40 s
Sample volume approx. 1 mL
Accuracy and ambient air pressure sensor | full range viscosity correction | reference
convenience features oscillator | automatic bubble detection | camera image of the measuring
cell
a According to ISO 5725
b Under ideal conditions and for low densities/viscosities
c Cooling down more than 20 °C (36 °F) below ambient temperature only with DMA M CK
d For the measuring cell together with the injection adapters DMA/CarboQC (mat. no. 159537) in the temperature range of
0–50 °C (32–122 °F). For temperatures above 50 °C (122 °F), the maximum allowed pressure is 5 bar (72.5 psi) absolute
pressure. See also section 8.9.
e After full temperature equilibrium

Table 9: Precisiona of concentration measurements under repeatability conditions (aqueous solutions, % w/w)

DMA 4100 M DMA 4500 M DMA 5000 M


b
Ethanol 0.05 0.025 < 0.01
Extract/Sugar 0.025 0.015 < 0.01
HCl 0.02 0.01 < 0.01
NaOH 0.04 0.02 < 0.01
H3PO4 0.06 0.03 < 0.01
HNO3 0.07 0.035 < 0.01
H2SO4 0.05 0.025 < 0.01
a The accuracy is not the same over the whole concentration range. The values given are typical values for orientation purposes.
b In the temperature range 15–25 °C (59–77 °F) the accuracy is 0.01 % w/w.

XDLIB016EN-K 47
Appendix A: Technical Data

Table 10: Precision classes

Precision class Stability temperature Stability density


Ultrafast < 0.1 °C for 10 s < 0.000005 g/cm3 for 15/45 s a
Fast < 0.05 °C for 10 s < 0.000005 g/cm3 for 60 s
Standard < 0.005 °C for 10 s < 0.000005 g/cm3 for 60 s
Precise < 0.002 °C for 10 s < 0.000001 g/cm3 for 60 s
a 45 s for temperature scans

A.2: Instrument Data and Operating Conditions


Environmental conditions indoor use only
(EN 61010)
Ambient temperature 15 °C to 35 °C (59 °F to 95 °F)
Air humidity 10 % to 90 % relative humidity, non-condensing
Altitude max. 3000 m (9800 ft)
Pollution degree 2
Overvoltage category II
Memory 1000 measuring values with / without camera pictures
Touchscreen 10.4" TFT PCAP touchscreen 640 x 480 px
Interfaces 4 x USB (2.0 full speed), 1 x Ethernet (100 Mbit), 1 x RS-232,
1 x CAN Bus, 1 x VGA
RS-232C printer settings Baud rate: 9600; Parity: none; Stop bit: 1; Data bits: 8
Voltage 100 to 240 V~, 50/60 Hz, fluctuation ±10 %
Power consumption 190 VA (incl. Xsample and external measuring modules)a
Power inlet according to IEC/EN 60320-1/C14, protection class I
Fuses ceramic tube fuses 5x20 mm; IEC60127-2; AC 250 V; T 5 AH
Dimensions (L x W x H) 495 mm x 330 mm x 230 mm (19.5 in x 13 in x 9 in)
Weight 22.5 kg (49.6 lbs)
Housing materials
Top & side cover aluminum, coated
Back aluminum
Front, Xsample slot cover plate polystyrene / butadiene
a In the stand-alone configuration (no Xsample or external measuring modules) the power consumption will not exceed 85 VA.

IMPORTANT: Connect only Anton Paar equipment


or equipment with a maximum power consumption
WARNING of 40 W to the CAN interface. Otherwise the instru-
ment will not work.
Risk of electric shock
Connect only devices that comply with PELV
(protective extra-low voltage) according to
EN 61140 or with SELV (safety extra-low voltage)
according to EN 60950 to any of the electrical
interface connectors of the instrument.

48 XDLIB016EN-K
Appendix A: Technical Data

A.3: Wetted Parts


The following materials are in contact with the samples and cleaning agents:

DMA M

Material Part
Borosilicate glass measuring cell
PTFE filling adapter

Standard accessories

Material Part
ETFE adapter UNF ¼" Luer male
Polyethylene waste vessel
Polypropylene/polyethylene syringe 2 mL Luer
PTFE adapter Luer cone, injection adapter Luer, male Luer plug PTFE,
filling and waste hose for DMA 5000 M
Silicone hose

XDLIB016EN-K 49
Appendix B: Output Quantities and Live Raw Data

Appendix B: Output Quantities and Live Raw Data


B.1: Output Quantities
The following quantities can be selected as output for the output fields.

Group: Acid / Base Tables


Concentration of different aqueous acids and bases in percentage by weight (% w/w) and
mole per liter (mol/L) according to different tables.
Number of digits displayed for % w/w values: DMA 5000 M: 3 | DMA 4500 M: 2 | DMA 4100 M: 2
Number of digits displayed for mol/L and N values: DMA 5000 M: 4 | DMA 4500 M: 3 | DMA 4100 M: 3
Hydrochloric Acid (HCl) CRC Handbook of Chemistry and Physics, based on true density at
(% w/w) (mol/L) (N) 20 °C, range 0–40 % (0–21.5 mol/L). Accuracy approx. 0.02 %
(0.01 mol/L)
Nitric Acid (HNO3) Landolt-Boernstein, based on true density at 20 °C, range 0–100 % (0–
(% w/w) (mol/L) (N) 23.9 mol/L). Accuracy approx. 0.07 % (0.02 mol/L)
Phosphoric Acid (H3PO4) Landolt-Boernstein, based on true density at 20 °C, range 0–100 % (0–
(% w/w) (mol/L) (N) 19.03 mol/L). Accuracy approx. 0.06 % (0.01 mol/L)
Sodium Hydroxide (NaOH)a Landolt-Boernstein, based on true density at 20 °C, range 0–50 % (0–
(% w/w) (mol/L) (N) 19 mol/L). Accuracy approx. 0.04 % (0.01 mol/L)
Sulfuric Acid (H2SO4) CRC Handbook of Chemistry and Physics, based on true density at
(% w/w) (mol/L) (N) 20 °C, range 0–94 % (0–17.6 mol/L). Accuracy approx. 0.05 %
(0.01 mol/L)
a Notice: Corrodes measuring cell.

Group: API Functions


The API functions automatically convert the density values of petroleum samples measured at any tem-
perature to density, API gravity or specific gravity at 15 °C or 60 °F, according to ASTM D1250-08 and
DIN 51757. Additionally, the same API functions are available for a reference temperature of 20 °C
according to the IP Petroleum Measurement Paper No. 3, 1988.
The samples are divided into the groups crude oil (group A), fuel to heating oil (group B), and lubricants
(group D).
Number of digits displayed for API density values: DMA 5000 M: 5 | DMA 4500 M: 5 | DMA 4100 M: 4
Number of digits displayed for °API Gravity values: DMA 5000 M: 3 | DMA 4500 M: 2 | DMA 4100 M: 2
°API Gravity 15 °C
°API Gravity 20 °C
API gravity converted to 15 °C | 20 °C | 29.5 °C | 60 °F
°API Gravity 29.5 °C
°API Gravity 60 °F
API Density 15 °C
API Density 20 °C Conversion of density at measuring temperature to
API Density 29.5 °C density at 15 °C | 20 °C | 29.5 °C | 60 °F
API Density 60 °F
API Input Quantity Selection of the input parameter for API calculations: Density, Density
(not visc.-corr.), or a special adjustment
API Product Group Selection of the API product group for calculation of API gravity,
density, and specific gravity

50 XDLIB016EN-K
Appendix B: Output Quantities and Live Raw Data

Group: API Functions (cont.)


API Specific Gravity 15 °C
API Specific Gravity 20 °C Conversion of density at measuring temperature to
API Specific Gravity 29.5 °C specific gravity at 15 °C | 20 °C | 29.5 °C | 60 °F
API Specific Gravity 60 °F

Group: Density
Number of digits displayed for density values: DMA 5000 M: 6 | DMA 4500 M: 5 | DMA 4100 M: 4
Number of digits displayed for temperature values: DMA 5000 M: 3 | DMA 4500 M: 2 | DMA 4100 M: 2
Apparent Density Brass Apparent density referring to scales adjusted with brass weights
Apparent Density Steel Apparent density referring to scales adjusted with steel weights
Apparent Specific Gravity Apparent density divided by the apparent density of water at the spec-
ified temperature. Apparent density is the weight in air (not mass!)
divided by the volume.
Density Value of viscosity-corrected true density
Density (not visc.-corr.) Density value without viscosity correction. The density is correct for
samples with a viscosity at around 1 mPa·s (water). Noticeable high
readings for samples of higher viscosity.
Density Condition Current status of the measurement
Density Control Temp. Temperature in the cell block measured by the Pt 100 control sensor
Density Set Temp. Set measuring temperature
Density Temperature Temperature in the measuring cell measured by the Pt 100 measuring
sensor
Repeat Dev. Density Density deviation of two subsequent measurements; only available if
repeated mode is used and the quantity “Density” has been activated
Set Viscosity Entered viscosity [mPa·s] used for the manual viscosity correction
Specific Gravity Density of the sample at measuring temperature divided by the
density of water at measuring temperature
Specific Gravity (not visc.-corr.) Specific gravity without viscosity correction
Specific Gravity t/04 Density of the sample at measuring temperature divided by the
density of water at 4 °C

Group: Density (Expert)


d Density number, calculated by subtracting the density of water from
the measured density and dividing the result by the density of water at
measuring temperature
d (not visc.-corr.) Density number without viscosity correction
Damping Damping represents the energy loss during oscillation caused by
sample viscosity. Used for viscosity correction of the density.
Dynamic Viscosity Determined viscosity in mPa·s, Ns/m2 and Pa·s. Only suitable for
Newtonian fluids. Displayed range: 10 mPa·s to 3000 mPa·s (10 %
accuracy).
Last Air/Water at 20 °C Datea Date of the last air/water adjustment
Last Air/Water Adjustment Usera Name of the user who has performed the last air/water adjustment

XDLIB016EN-K 51
Appendix B: Output Quantities and Live Raw Data

Group: Density (Expert) (cont.)


Periodic Time Period of oscillation of the U-tube in the harmonic oscillation of 0th order
Periodic Time 1st Harmonic Period of oscillation of the U-tube in the harmonic oscillation of 1st order
Periodic Time Ref. Oscillator Actual period of oscillation of the reference oscillator
PQ U-tube Quotient of the period of oscillation of the U-tube divided by the period
of oscillation of the reference oscillator
PQ U-tube 1st Harmonic Quotient of the period of oscillation of 1st order of the U-tube divided
by the period of oscillation of the reference oscillator
Quality Factor Quality factor: 10000 divided by the damping value. Value equals the
damping value in software versions 2.92.204 and lower.
a Not available in non-storage mode

Group: Ethanol Tables


Ethanol concentrations in percentage by volume (% v/v) or percentage by weight (% w/w) according to
ethanol concentration tables issued by different organizations/authors
Number of digits displayed with ethanol values: DMA 5000 M: 3 | DMA 4500 M: 2 | DMA 4100 M: 2
Canadian Excise Alcohol Tablea Special ethanol table converting the output of a special adjustment into
an ethanol value
TIP: Before you use this output quantity, it is necessary to perform a
special adjustment with apparent density values of air and water, see
section 9.3.4.2, and to link that adjustment to the Canadian excise
alcohol table, see section 7.2.4.
Ethanol AOAC 60 °F (% v/v) Percentage by volume at 15.56 °C (60 °F), AOAC (American Organi-
zation of Analytical Chemists) tables, based on true density at 20 °C.
Measuring temperature must be 20 °C (68 °F).
Ethanol AOAC 60 °F (% v/v) Ethanol AOAC 60 °F (% v/v) without viscosity correction
(not visc.-corr.)
Ethanol HM C&E (% v/v) HM C&E table at 20 °C
Ethanol HM C&E (% w/w)
Ethanol IUPAC (% v/v) Tables of the International Union of Pure and Applied Chemistry, based
Ethanol IUPAC (% w/w) on true density at 20 °C. Measuring temperature must be 20 °C (68 °F).
Ethanol Kaempf (% v/v) Percentage by volume/weight according to W. Kaempf, based on true
Ethanol Kaempf (% w/w) density at 20 °C
Ethanol OIML (% v/v) According to the tables of the International Organization of Legal Metrol-
Ethanol OIML (% w/w) ogy (OIML), temperature according to ITS-68, based on true density at
20 °C
Ethanol OIML SHUSEI-DO Percentage by volume at 15 °C (59 °F), based on true density at 15 °C
1000 POINTS (% v/v) (59 °F). Measuring temperature must be 15 °C (59 °F).
Ethanol OIML ITS-90 (% v/v) According to the tables of the International Organization of Legal Metrol-
Ethanol OIML ITS-90 (% w/w) ogy (OIML), temperature according to ITS-90, based on true density at
20 °C
Ethanol Proof 60 °F Proof degrees at 15.56 °C (60 °F), based on true density at 20 °C
Ethanol Proof 60 °F Ethanol Proof 60 °F without viscosity correction
(not visc.-corr.)
a Not available in non-storage mode

52 XDLIB016EN-K
Appendix B: Output Quantities and Live Raw Data

Group: Extract / Sugar Tables


Concentration of extract/sugar (sucrose) of beverages in different concentration units
Number of digits displayed with concentration values: DMA 5000 M: 3 | DMA 4500 M: 2 | DMA 4100 M: 2
Number of digits displayed with Mass Concentration Sugar: all 3 models: 0 (mg/L), 1 (g/L, kg/m3), 4 (g/mL)
Baumé Based on specific gravity (SG) at set temperature
for liquids heavier than water: °Be = (145 x SG – 145) / SG
for liquids lighter than water: °Be = (140 – 130 x SG) / SG
Concentration Sugar (°Balling) Extract in percentage by weight, Balling table, based on true density
at 20 °C
Concentration Sugar (°Brix) Sucrose in percentage by weight, NBS Table 113, based on true
density at 20 °C
Concentration Sugar (°Plato) Extract in percentage by weight, Plato table, based on true density at
20 °C
Mass Concentration Sugar Sucrose in g/L, g/mL, mg/L, kg/m3
Nihonshu-Do (°) Based on specific gravity (SG) t/04 at 15 °C
Nihonshu-Do = 1443 / SG (15/4) – 1443

Group: Special Adjustmentsa


Up to 5 special adjustments can be stored in the instrument, see section 9.3.4.
a Not available in non-storage mode

Group: System
DataField1 Name of the user-defined data field (optional sample ID)
DataField2 Name of the user-defined data field (optional sample ID)
DataField3 Name of the user-defined data field (optional sample ID)
Date Current date
Instrument name Name of the instrument as defined in the general instrument settings
a
Last Check Date Date of the last GxP-relevant check
a
Last Check Name Name of the last GxP-relevant check
Last Check Resulta Result of the last GxP-relevant check
a
Last Check Type Type of the last GxP-relevant check
a
Last Check User Name of the user who has performed the last GxP-relevant check
Location Location of the instrument as defined in the general instrument settings
Master Condition Sum of all available conditions from measuring modules in the system
Measurement Mode Selected type of measurement, see section 7.2.3
Method Name of the selected or used method
Parent Sample Id Sample ID of the parent sample, used with measurement modes that
perform multiple measurements with the same sample
Sample Error State Error messages concerning the sample: “No error”, “Was canceled”, etc.
Sample Info Information on measurement mode, parent sample ID, and sub mea-
surement number
Sample List Number Number of the current sample list entry
Sample Name Name of the current sample

XDLIB016EN-K 53
Appendix B: Output Quantities and Live Raw Data

Group: System (cont.)


Serial Number Serial number of the instrument
Stability Status Two-digit number indicating the reached stability criteria. The first digit
represents temperature stability, the second digit, density stability.
Sub Measurement Number Sub measurement numbers are available if multiple measurements /
determinations are performed with the same sample.
Time Current time
Unique Sample Id Internal unique sample ID, which cannot be reset
User Name of the user in a certain context
a Not available in non-storage mode

Group: User Functions


User functions can be constants, formulas, linear functions, polynomials (1D or 2D), tables, or
measurement mode functions (see General Software Functions Manual, section 9.2).

B.2: Live Raw Data


For viewing and printing live raw data as well as for a list of software-specific live raw data, refer to the
General Software Functions Manual, section 10.9.

DMA Density
Quantities not listed in the following table are described in the tables above (e.g. Density, Density Tempera-
ture, Density (not visc.-corr.), etc.).

Delta RHO Value Difference between density calculated from 1st harmonic and density
calculated from fundamental oscillation
Density Forecast Pre-calculated density at the set temperature
Density Progress Indicator (0–100) for the progress of the measurement
Fill Status Status information about correct filling of the U-tube
Values different from zero indicate an incorrect filling.
RHO NC Fundamental Value Not viscosity-corrected density calculated from the fundamental oscillation
RHO NC Harmonic Value Not viscosity-corrected density calculated from the 1st harmonic
RHO VC Fundamental Value Viscosity corrected density calculated from the fundamental oscillation
RHO VC 1st Harmonic Viscosity corrected density calculated from the 1st harmonic of the U-tube

DCB – Air Pressure

Air Pressure Currently measured air pressure


Air Pressure Condition Current status of the measurement
Air Pressure State Status of the air pressure measurement
Air Pressure Substate Detailed information about the status of the air pressure measurement

54 XDLIB016EN-K
Appendix C: List of Quick Settings Parameters

Appendix C: List of Quick Settings Parameters


Depending on the sample list mode, different quick setting parameters are set by default:
• If the “No Sample List” mode is used: • If the “Sample List” mode is used:
Sample name, measurement mode and Measurement mode and “Density Temperature”
“Density Temperature” (not for users of the user (not for users of the user group “Operator”)
group “Operator”)

Table 11: Quick settings parameters

Parameter Type Parameter Select Description


Sample Name only in the “No Sample List” mode
Measurement Mode S (Standard) Perform a standard measurement.
C (Check) Perform one of the predefined checks. It is
only possible to select a check that has been
defined for the selected method before.
MM (Multiple Measurement) Perform 2–10 measurements of a single
sample automatically.
RM (Repeated Mode) Perform repeated measurements of a single
sample by filling the sample up to 5 times.
You define a maximum deviation of two
subsequent measurements.
MF (Multiple Filling) Perform multiple measurements of a single
sample after filling the sample 2–10 times.
TS (Temperature Scan) Perform a temperature scan.
TTS (Temperature Table Scan) Perform a temperature table scan.
Density Temperature Set the temperature of the density mea-
suring cell between –25 °C and 100 °C
(or 95 °C or 90 °C).
Density Precision Class Ultrafast
Fast (all models)
Standard (default)
Precise (for DMA 5000 M)
None (use method default)
Density Measurement Set the time for the measurement delay
Delay (0–600 s).
Density Timeout Set the timeout for density measurement
(30–3600 s, default 600 s).
Density FillingCheck™ Always active default
Not active
Active during measurement
None (use method default)
Density Stability criterion Prerequisite for precision class “Ultrafast”

XDLIB016EN-K 55
Appendix C: List of Quick Settings Parameters

Table 11: Quick settings parameters (cont.)

Parameter Type Parameter Select Description


Density A - Crude oil default
API Product Group B - Fuels
D - Lubes
None (use method default)
Density Density default
API Input Quantity Density (not visc.-corr.)
Special Adjustmenta up to 5
None (use method default)
Density Canadian Excise Special Adjustment 1, …, 5 default
Alcohol Tablea None (use method default)
User-defined data fields if set as mandatory in the sample list settings
User functions of the if activated in the method settings
“Constant” type
a Not available in non-storage mode

56 XDLIB016EN-K
Appendix D: Density Tables

Appendix D: Density Tables


IMPORTANT: The factory default reference values for the density of air and water are based on the formula
of Spieweck/Bettin and cover the whole measuring range of the instrument.

D.1: Density of Air


Formula for the calculation of the density of air by The numbers are valid for a CO2 content in air of
Spieweck/Bettin1 (simplified equation; given an air 0.04 % v/v; change ρ by ±1/19000 for every change
humidity of 50 %): in CO2 volume content of ±0.0001.
Composition of dry air [% v/v]:
0.34844  p – 0.5   0.252  t – 2.0582 
 = --------------------------------------------------------------------------------------------------  1000 78.110 % N2
273.15 + t
20.938 % O2
ρ.... density [g/cm3] 0.916 % Ar
t..... temperature [°C] 0.033 % CO2
p.... pressure [hPa] 0.002 % Ne

Table 12: Density of air [g/cm3] according to Spieweck/Bettin

Temperature Density at the pressure [hPa]


[°C] 900 920 940 960 980 1000 1013.25 1050
–10 0.001200 0.001227 0.001253 0.001280 0.001306 0.001333 0.001350 0.001399
–5 0.001176 0.001202 0.001228 0.001254 0.001280 0.001306 0.001323 0.001371
0 0.001152 0.001177 0.001203 0.001228 0.001254 0.001279 0.001296 0.001343
5 0.001129 0.001154 0.001179 0.001204 0.001229 0.001254 0.001271 0.001317
10 0.001107 0.001131 0.001156 0.001181 0.001205 0.001230 0.001246 0.001291
15 0.001085 0.001110 0.001134 0.001158 0.001182 0.001206 0.001222 0.001267
20 0.001065 0.001088 0.001112 0.001136 0.001160 0.001184 0.001199 0.001243
25 0.001045 0.001068 0.001091 0.001115 0.001138 0.001162 0.001177 0.001220
30 0.001025 0.001048 0.001071 0.001094 0.001117 0.001140 0.001156 0.001198
35 0.001007 0.001029 0.001052 0.001075 0.001097 0.001120 0.001135 0.001176
40 0.000989 0.001011 0.001033 0.001055 0.001078 0.001100 0.001115 0.001156
45 0.000971 0.000993 0.001015 0.001037 0.001059 0.001081 0.001095 0.001135
50 0.000954 0.000976 0.000997 0.001019 0.001040 0.001062 0.001076 0.001116
55 0.000938 0.000959 0.000980 0.001001 0.001023 0.001044 0.001058 0.001097
60 0.000922 0.000943 0.000964 0.000984 0.001005 0.001026 0.001040 0.001079
65 0.000906 0.000927 0.000947 0.000968 0.000989 0.001009 0.001023 0.001061
70 0.000891 0.000911 0.000932 0.000952 0.000972 0.000993 0.001006 0.001043
75 0.000877 0.000897 0.000917 0.000937 0.000957 0.000977 0.000990 0.001027
80 0.000862 0.000882 0.000902 0.000922 0.000941 0.000961 0.000974 0.001010
85 0.000849 0.000868 0.000887 0.000907 0.000926 0.000946 0.000959 0.000995
90 0.000835 0.000854 0.000874 0.000893 0.000912 0.000931 0.000944 0.000979
95 0.000822 0.000841 0.000860 0.000879 0.000898 0.000917 0.000929 0.000964
100 0.000809 0.000828 0.000847 0.000865 0.000884 0.000903 0.000915 0.000949

1 F. Spieweck, H. Bettin: Review: Solid and liquid density determination. tm – Technisches Messen 59 (1992) 7–8,
pp. 285–292.

XDLIB016EN-K 57
Appendix D: Density Tables

D.2: Density of Water (0 °C to 100 °C)


Formula for the calculation of the density of water (ρ = density / t = temperature)
• according to Spieweck/Bettin:
5
n
n = 0 an  t
  t  = ----------------------------------
1+bt

a0 = 9.998 395 2·102 kg/m3


a1 = 1.695 257 7·101 °C–1 kg/m3
a2 = –7.990 512 7·10–3 °C–2 kg/m3
a3 = –4.624 175 7·10–5 °C–3 kg/m3
a4 = 1.058 460 1·10–7 °C–4 kg/m3
a5 = –2.810 300 6·10–10°C–5 kg/m3
b = 1.688 723 6·10–2 °C–1

• according to CIPM:

2
 t + a1    t + a2 
  t  = a 5  1 – ---------------------------------------------
a3   t + a4 

a1 = –3.983 035 °C
a2 = 301.797 °C
a3 = 522 528.9 °C2
a4 = 69.348 81 °C
a5 = 999.974 950 kg/m3

58 XDLIB016EN-K
Appendix D: Density Tables

Table 13: Density of water [g/cm3] at temperature T [°C]

T IAPWS-95/ Spieweck/ T IAPWS-95/ Spieweck/ T IAPWS-95/ Spieweck/


[°C] CIPM Bettin [°C] CIPM Bettin [°C] CIPM Bettin
0 0.999843 0.999840 40 0.992216 0.992212 80 0.971790 0.971785
1 0.999902 0.999899 41 0.991830 0.991826 81 0.971165 0.971159
2 0.999943 0.999940 42 0.991437 0.991432 82 0.970534 0.970528
3 0.999967 0.999964 43 0.991036 0.991031 83 0.969898 0.969892
4 0.999975 0.999972 44 0.990628 0.990623 84 0.969257 0.969252
5 0.999967 0.999964 45 0.990213 0.990208 85 0.968611 0.968606
6 0.999943 0.999940 46 0.989791 0.989786 86 0.967961 0.967955
7 0.999904 0.999901 47 0.989362 0.989358 87 0.967305 0.967300
8 0.999851 0.999848 48 0.988926 0.988922 88 0.966645 0.966639
9 0.999784 0.999781 49 0.988484 0.988479 89 0.965980 0.965974
10 0.999702 0.999699 50 0.988035 0.988030 90 0.965310 0.965304
11 0.999608 0.999605 51 0.987579 0.987575 91 0.964635 0.964630
12 0.999500 0.999497 52 0.987117 0.987113 92 0.963955 0.963950
13 0.999380 0.999377 53 0.986649 0.986644 93 0.963271 0.963266
14 0.999247 0.999244 54 0.986174 0.986169 94 0.962582 0.962577
15 0.999103 0.999099 55 0.985693 0.985688 95 0.961888 0.961883
16 0.998946 0.998942 56 0.985206 0.985201 96 0.961189 0.961185
17 0.998778 0.998774 57 0.984712 0.984707 97 0.960486 0.960482
18 0.998599 0.998595 58 0.984213 0.984208 98 0.959778 0.959774
19 0.998408 0.998404 59 0.983707 0.983702 99 0.959066 0.959062
20 0.998207 0.998203 60 0.983196 0.983191
21 0.997995 0.997991 61 0.982678 0.982673
22 0.997773 0.997769 62 0.982155 0.982150
23 0.997541 0.997537 63 0.981626 0.981621
24 0.997299 0.997295 64 0.981091 0.981086
25 0.997048 0.997043 65 0.980551 0.980546
26 0.996786 0.996782 66 0.980005 0.979999
27 0.996516 0.996511 67 0.979453 0.979448
28 0.996236 0.996232 68 0.978896 0.978890
29 0.995947 0.995943 69 0.978333 0.978327
30 0.995649 0.995645 70 0.977765 0.977759
31 0.995343 0.995339 71 0.977191 0.977185
32 0.995028 0.995024 72 0.976612 0.976606
33 0.994705 0.994700 73 0.976028 0.976022
34 0.994373 0.994369 74 0.975438 0.975432
35 0.994033 0.994029 75 0.974843 0.974837
36 0.993685 0.993681 76 0.974243 0.974237
37 0.993330 0.993325 77 0.973637 0.973632
38 0.992966 0.992962 78 0.973027 0.973021
39 0.992595 0.992591 79 0.972411 0.972405

XDLIB016EN-K 59
Appendix E: List of Typical Samples and Recommended Cleaning Liquids

Appendix E: List of Typical Samples and


Recommended Cleaning Liquids
Suggested Suggested
Sample
cleaning liquid 1 cleaning liquid 2
After-shave, perfume alcohol
(e.g. ethanol 96 %),
acetone
Alcohols e.g. ethylene glycol, warm water, alcohol (e.g. ethanol 96 %),
propylene glycol, ethanol 96 % acetone
glycerol, mixtures
(e.g. antifreeze)
Alcoholic beverages e.g. alcopops, beer, water, alcohol (e.g. ethanol 96 %)
cider, gin, spirits, enzymatic lab cleanera
sparkling wine, wine
malt, wort water, alcohol (e.g. ethanol 96 %)
enzymatic lab cleanera
Edible oils petroleum naphtha, alcohol (e.g. ethanol 96 %),
hexane, isohexane acetone
Fuel petroleum naphtha alcohol (e.g. ethanol 96 %),
acetone
e.g. diesel fuel, petroleum benzine, alcohol (e.g. ethanol 96 %),
biodiesel, kerosene, petroleum ether, acetone
aviation gasoline, petroleum naphtha,
light heating oils white spirit, pentane,
heptane, cyclohexane,
nonane
Heavy oil samples e.g. crude oils, toluene, petroleum alcohol (e.g. ethanol 96 %),
heavy crude oils naphtha, white spirit acetone
Hydraulic fluids mineral oil based petroleum benzine,
petroleum ether,
petroleum naphtha,
heptane, white spirit
silicone oil based xylene, toluene petroleum benzine,
heptane, petroleum ether
Liquid soap & detergent water alcohol (e.g. ethanol 96 %)
Lubricating oil & petroleum naphtha alcohol (e.g. ethanol 96 %),
other fresh oils acetone
fresh lube oils incl. gear petroleum benzine, alcohol (e.g. ethanol 96 %),
oils, oils for industrial toluene, xylene, acetone
machinery, automatic mesitylene
transmission fluid
(ATF), transformer oils,
heat transfer oils, oils
for conservation and
corrosion protection

60 XDLIB016EN-K
Appendix E: List of Typical Samples and Recommended Cleaning Liquids

Suggested Suggested
Sample (cont.)
cleaning liquid 1 cleaning liquid 2
Milk, cream water, dish washing alcohol (e.g. ethanol 96 %)
agent in water,
enzymatic lab cleanera
Motor oil petroleum naphtha alcohol (e.g. ethanol 96 %),
acetone
Nonalcoholic beverages orange juice, syrup, (warm) water, dish alcohol (e.g. ethanol 96 %)
soft drinks washing agent in water
Salad dressing, petroleum naphtha, alcohol (e.g. ethanol 96 %)
mayonnaise dish washing agent in
water
Schnapps alcohol
(e.g. ethanol 96 %)
Shampoo water alcohol (e.g. ethanol 96 %)
Suntan lotion petroleum naphtha, alcohol (e.g. ethanol 96 %)
dish washing agent in
water
Waxes, paraffin-type toluene, petroleum alcohol (e.g. ethanol 96 %),
samples naphtha, white spirit acetone
Wood protection / petroleum naphtha alcohol (e.g. ethanol 96 %)
white spirit based (water)
(water-based)
a Using an enzymatic lab cleaner is recommended for special cleaning. After using the lab cleaner, you need to rinse the
measuring cell with water.

To prevent limestone deposits, never use tap water We recommend Winepress Cleaner PM Membrane
as the cleaning liquid 2. Use ultra-pure water Presses, cat. no. 409004, by Wigol® or TM Desana
instead. by Thonhauser. Refer to the instructions of the
manufacturer concerning the concentration of the
Strong alkaline lab cleaners (pH > 10.5) should only
cleaning agent.
be applied briefly and at temperatures below 25 °C
because strong bases attack the glass surface upon Some samples that contain proteins, e.g. beer or
prolonged exposure and at high temperatures. wort, may cause residues in the measuring cell after
longer measurement periods. In this case use an
enzymatic lab cleaner to remove the residues from
the cell.
Do not use cleaners with abrasives.

XDLIB016EN-K 61
Appendix F: Troubleshooting

Appendix F: Troubleshooting
Table 14: Adjustment

Problem Cause / Corrective action see


Readjustment is necessary Bad water quality for checks/adjustments: section 9.3.1
very often. - Use freshly degassed ultra-pure water.
The measuring cell is not clean: section 10
- Clean and dry the measuring cell perfectly before an air
check/adjustment.
The measuring cell is corroded by hydrofluoric acid, strong section 10
alkaline solutions or mechanical abrasion:
- Do not leave glass-corroding liquids in the measuring cell.
Direct sunlight on the instrument: section 4.1
- Install the DMA M at a place without direct sunlight.
The adjustment is still not The measuring cell is not sufficiently dry for the air adjustment: section 10
finished after 10 minutes. - Clean and dry the measuring cell perfectly before an air
check/adjustment.
There are gas bubbles in the measuring cell during water section 9.3.1
adjustment:
- Repeat the filling procedure and use freshly degassed
ultra-pure water.

Table 15: Measurement

Problem Cause / Corrective action see


I cannot start any measure- - Check if any module has a firmware version installed that General
ment 15 minutes or more is older than expected by the instrument’s software. The Software
after booting the instru- information is either displayed on the start screen or in the Functions
ment. message list of the quick access area. Manual,
- Tap <Menu> and select Service > Update > Module section 10.4
Firmware Update to update any modules using the
internal firmware update package.
Density Condition: One or more samples are highly viscous. This may lead to a
“Filling Warning” filling warning as shown.
Gas bubbles in the measuring cell: section 8.6
- Degas your sample. Fill the sample with a higher tempera-
ture than the measuring temperature.
Density Condition: The measuring cell is only partly filled:
“Error: No Oscillation” - Fill the sample again.
Density Condition: The sample is instable (e.g. emulsion): section 8.7
“Error: Timeout” - Preheat / precool your sample to measuring temperature.
The timeout is set too short: section 7.2.1
- Change the timeout setting.
The instrument cannot reach the criteria for the set precision appendix B
class, e.g. due to the presence of air bubbles or particles in
the cell.
- Check the “Stability status” of the measurement.
Only for DMA 4100 M (mat. no. 163378, 176251, or 176802),
DMA 4500 M (mat. no. 176803, 176804, or 176805) and
DMA 5000 M (mat. no. 182706, 186723 or 185098).

62 XDLIB016EN-K
Appendix F: Troubleshooting

Table 15: Measurement (cont.)

Problem Cause / Corrective action see


The calibration failed. Bad cleaning and drying: section 10.1
The results deviate from - Improve your cleaning and drying procedure.
reference values. The calibration liquid has been stored too long:
- Use a fresh calibration liquid.
Adjustment problems: section 9.3.1
- Improve your adjustment routine.
Error message: • Glass cell could be broken.
“Broken U-tube” • This error might also appear due to inhomogeneous filling.
If it persists, do not fill any liquids, switch off the instrument,
and contact your local Anton Paar representative.

Table 16: Touchscreen

Problem Cause / Corrective action see


The screen elements do not Bad touchscreen calibration: General
react when tapped. - Perform a new touchscreen calibration. Software
Functions
Manual,
section 4.3
Only for instruments with 6.4" display:
- Exchange the protection foil (mat. no. 81233).
The screen flickers. Due to manufacturing tolerances of the hardware, the screen General
may flicker for certain values of reduced display brightness. Software
- Change the display brightness. Functions
Manual,
section 4.4

Table 17: Data memory

Problem Cause / Corrective action see


I cannot see certain results The filter function is activated, and the results do not match General
in the data memory. the filter criteria: Software
- Change the filter settings. Functions
Manual,
section 8.4
I have deleted all results The filter settings in menu “Delete Measured Data” are General
but there are still results different from the settings in menu “Data Browser Settings”: Software
visible in the data memory. - Perform corresponding settings in both menus. Functions
Manual,
section 8.7,
section 8.4

XDLIB016EN-K 63
Appendix F: Troubleshooting

Table 18: Data export

Problem Cause / Corrective action see


The export to the USB The USB memory device has the old super floppy formatting
memory device does not and is therefore not accepted by the instrument:
work. - Reformat with FAT32 or try a newer USB memory device.
Wrong output data are The settings in the menu “Result Output” are wrong: General
exported. - Change the settings. Software
Functions
Manual,
section 7.2.3

Table 19: Password protection

Problem Cause / Corrective action see


The instrument boots up A user with activated auto logon function was logged in on General
without logon procedure, the instrument before it was switched off: Software
and no password is - Tap on the user indicator icon and log on with another user Functions
requested. account. Manual,
section 6.5.2

Table 20: Printout problems

Problem Cause / Corrective action see


No printout on office printer Office printer problems:
- Check that the printer has enough paper, toner, etc.
See the corresponding printer manual.
The office printer type is not supported by your instrument. General
Wrong interface used: Software
- Use the interface that has been defined in menu “Printer Functions
Management” or change the interface settings. Manual,
section 5.3
Wrong or no definition of the printer in menu “Printer Manage-
ment”:
- Change the definition.
No printout on RS-232 Printer problems:
printer - Check the printer.
See the corresponding printer manual.
Wrong or no definition of the printer in menu “Printer Manage- General
ment”: Software
- Change the definition. Functions
Chinese printer: Manual,
- Declare the printer as “RS-232 (Chinese)” in menu section 5.3
“Printer Management”.
The printout on an RS-232 Wrong communication settings on the RS-232 printer: appendix A.2
printer makes no sense. - Change the DIP switch settings (see the printer manual).
Wrong output values are The settings in menu “Result Output” are wrong: General
printed. - Change the settings. Software
Functions
Manual,
section 7.2.3

64 XDLIB016EN-K
Appendix G: Menu Tree

Appendix G: Menu Tree


The coloring of the menu tree indicates which Administrator
parts of the menu are accessible for users with
Administrator, Manager
administrator, manager, or operator rights:
Administrator, Manager, Operator

Checks/Adjustments Checks
Air/Water at 20 °C
Other Adjustments Density Module Air / Water at 20 °C
Air / Water Wide Range
Special Adjustments
Reset To Factory Adjustment
DCB Module Atmospheric Pressure Sensor
Adjustment
Data Memory Measured Dataa
Delete / Archive Measured
Dataa b
Statistica
Check Dataa
Delete / Archive Check
Dataa b
Adjustment Dataa Density Module Density Adjustment
Temperature Adjustment
Density Adjustment Trend
Special Adjustment
DCB Module Atmospheric Pressure Sensor
Adjustment
Print or Export Adjustment Data
Audit Trail
Delete Audit Trailc
Methods Method Settings Density (Current Method) Activate Modules / Constants
Activate Functionsd
Measurement Mode (S)
Repeated Mode Settings
Density Module
Display Layout
Result Output
Limits
Formula Parameters
Quick Settings Management
Density (not visc.-corr.)
°Brix
Ethanol (% w/w OIML-ITS90)
Ethanol (% v/v OIML-ITS90)
Ethanol (°Proof 60 °F AOAC)
Crude Oil (API)
Fuel Oil (API)
Lubricants (API)
Sulfuric Acid (% w/w)
Method Management
Method Visibility

XDLIB016EN-K 65
Appendix G: Menu Tree

Setup Measuring System Settings Density Module


Sample List Sample List / Sample Settings
User-defined Data Fields
Sample List Warnings
Mandatory Data Fields
Camera
Air Pump
Temperature Extrapolation Settings
Control Panel Date and Time
Regional Settings
Time Server Settings
Input Units
Printer Management
Network
External Interface Settings
Instrument Name and Location
Screen Saver
Sound Settings
VNC Settings
Calibrate External Touch Screen
Keyboard and Bar Code Settings
FTP Settings
Advanced Camera Settings
SMTP Server Settings
Display Brightness
System Security Security Level
Non Storage Mode
Value Visibility
Audit Trail
Electronic Signaturea
Logon Settings
Increased Security
Advanced Security
Unlock Service
User Managemente User Administration
User Group Administration
Printout Settings Automatic Printout
Report Management
Select Logos
Import Logos
Name and Address
Data Browser Settingsa
Expert Settings User Function Management
Measurement Mode Functions
Delete Functions
Calculator
Group Calculator
Check Management
Data Memory Settingsf

66 XDLIB016EN-K
Appendix G: Menu Tree

Service Backup Instrument Settings


Restore Instrument Settings
Update System Update
Module Firmware Update
Install Language Pack
Logging Configuration
System Information
IQ/OQ Report
Export Instrument Data
Switch to Desktop-Mode
Full System Backup
Full System Restore
Live Raw Data DMA Density
Calculations
DCB - Air Pump
DCB - Air Pressure
DCB - Environment
Reset to Factory Settings

a Not available in non-storage mode (for detailed information see the General Software Functions Manual, section 9.1.2)
b Depends on the Advanced Data Integrity settings
c Not available in the Advanced Data Integrity mode
d Only available if a measurement mode function is available
e Users of any user group may change their own password.
f Not available in non-storage mode (for detailed information see the General Software Functions Manual, section 9.1.2) and
in the Advanced Data Integrity mode

XDLIB016EN-K 67
Appendix H: EU Declaration of Conformity

Appendix H: EU Declaration of Conformity

68 XDLIB016EN-K

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