Cloud and Pour

7/24/2019 Cloud and Pour

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201051 sm INSTRUCTIONS FOR USE 16-2372-E / 13-2418-E

CAPP

Cloud and Pour Point

Refrigerator Bench -68C

ASTM D 97; ASTM D 2500; ASTM D 5853

IP 15; IP 219; DIN EN 23015

CFPP

Cold Filter Plugging Point

Refrigerator Bench -68C

ASTM D 6371; DIN EN 116; IP 309

SIS 155 122 (former DIN 51 428)

Quality Management System

The Petrotest GmbH Quality Management System:

Design, Manufacture, Sale and Repair of Petroleum Testing Devicesand Consistency Testing Devices according to the RequirementsDIN EN ISO 9001:2008. Certification Number 01 100 005115

Petrotest GmbH

A company of Anton Paar

Ludwig-Erhard-Ring 1315827 Dahlewitz - Germany

Phone: +49 (0)33708 56-300

Fax: +49 (0)33708 56-556

E-Mail: [email protected]: www.petrotest.com


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TABLE OF CONTENTS

1. Important Notes ........................................................................................................................ 4

1.1. Liability ................................................................................................................................. 4

1.2. Warranty ............................................................................................................................... 4

1.3. Service ................................................................................................................................. 5

1.4. General Safety Information ................................................................................................... 5

1.5. Device-specific Safety Information ........................................................................................ 6

1.6. Summary of all Warnings in this Document .......................................................................... 6

2. Technical Specifications of the Device ................................................................................... 7

3. Device Parts .............................................................................................................................. 7

4. Bringing into Service ................................................................................................................ 8

4.1. Preselection of the cooling temperature at the controller ...................................................... 9

5. Scope CAPP ............................................................................................................................ 10

5.1. Accessories CAPP ............................................................................................................. 10

5.2. Spare Parts CAPP .............................................................................................................. 10

6. ASTM D 97 ............................................................................................................................... 11

6.1. Procedure ........................................................................................................................... 11

6.2. Calculation and Report ....................................................................................................... 13

6.3. Precision and Bias .............................................................................................................. 13

7. ASTM D 2500 ........................................................................................................................... 14

7.1. Procedure ........................................................................................................................... 14

7.2. Report ................................................................................................................................ 16


8. Scope CFPP ............................................................................................................................ 17

8.1. Accessories CFPP .............................................................................................................. 17

8.2. Spare Parts CFPP .............................................................................................................. 18

9. ASTM D 6371 ........................................................................................................................... 18

9.1. Procedure ........................................................................................................................... 20



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1. IMPORTANT NOTES

1.1. Liability

The device is an electrically operated appliance. It may not be operated unattended or in

areas at risk of explosion or damp locations. Whenever the device is used, a thorough

knowledge of the Instructions for Use and compliance with same is assumed. In all cases the

operator is liable for the safe operation of the device if it is not used according to instructions.

Repair of the device must be carried out only by Petrotest GmbH. Only original Petrotest

parts and replacement parts must be used to operate the device.

Petrotest is not responsible for damage or malfunctions caused by the operator using the

device improperly or contrary to the instructions. We reserve the right to make technical

changes.

Caution

This device is not to be used in explosive atmospheres!

1.2. Warranty

1. Petrotest products are warranted against defects in material and workmanship for a

period of one year from the date of purchase.

2. Petrotest will replace or repair products - free of any charge - that fail as a result of

defective materials or workmanship within the warranty period.

3. None of the obligations of Petrotest shall apply to any products which have been

subjected to misuse, neglect, accident or any extreme environmental condition or

improper handling.

4. If defective products are returned to Petrotest, the costs of such return will be borne by

the customer, and those of delivering the repaired or replacement products to the

customer will be borne by Petrotest.

Petrotests sole liability shall be to repair or replace any product which proves to be defective.In no event shall Petrotest be liable for any special incidental, consequential, indirect or other

similar damages arising from failure of its products.


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1.3. Service

Should you require service, please contact our service department:

Petrotest GmbHA company of Anton Paar

Ludwig-Erhard-Ring 13

15827 Dahlewitz - Germany

Phone: +49 (0)33708 56-300Fax: +49 (0)33708 56-556

E-Mail: [email protected]

Website: www.petrotest.com

1.4. General Safety Information

1. The device should only be used by trained personnel or those who have been instructed

accordingly.

2. Alterations on the device, especially opening of same or changes to the electrical

connections/electronic devices should only be done by company trained service

technicians and only after receiving permission from Petrotest GmbH.

3. Unauthorized changes will also cause refusing warranty issues by Petrotest.

4. Before opening the device, disconnect the electrical current.

5. If heating devices are used, please ensure that there are no combustible materials near

the heating source.

6. For safety reasons, we recommend using an earth leakage circuit breaker. Ask your

electrician for further details and equipment.

7. We make these recommendations on the assumption that a regular function and safety

test is performed at least every two years.

8. Do not dispose of the device in ordinary household waste! In light of the long lifespan of

the device, regulations may change. For this reason, please only delegate the disposal of

the device to qualified personnel or speak to Petrotest!

For EU countries:

Directive 2002/96/EC: Directive 2002/96 of the European Parliament and of

the Council of 27 January 2003 on waste electrical and electronic

equipment. (Petrotest Registration Number WEEE 80418806).

The directive describes the obligation to not dispose of electrical and

electronic devices as unsorted municipal waste and to collect this WEEEseparately. Contact us for an authorized waste disposal company in your

country.

The product described in these instructions conforms with:

EC Low-Voltage Directive 73/23/EEC and 93/68 EEC respectively.

EMC Directive 2004/108/EC.


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1.5. Device-specific Safety Information

The apparatus doesn't constitute a potential danger for the operators that use it or for what

operate in the zones surrounding; notwithstanding this, we beg to follow the indications

below.

1. Avoid leaning any kind of material on the apparatus.2. Operators without qualification must not approach the operating

area.

3. Always wear suitable garments.

4. Always use masks, protective glasses and gloves conforming tothe normative in force.

5. Avoid sending water-spout on the device.6. Always pay attention to use of the apparatus.

7. It is severely forbidden to smoke next to the apparatus.

1.6. Summary of all Warnings in this Document

1. When setting up the device select a location away from heat, smoke, electrical or

magnetic interference and avoid excessive electrostatic discharges (ESD) to the device.

The bench top must be a level surface and free of vibration.

2. The device is tested to comply with the limits of the European Electromagnetic

Compatibility (EMC) Directive 2004/108/EC. However this device generates radio

frequency energy. If the device is not installed or used in accordance with the instruction

manual it may cause interference to radio communications.

3. Ensure the heater of the device is not exposed to flammable liquids or other combustible

material including the packaging material. Clean the surface before starting a heater test.


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2. TECHNICAL SPECIFICATIONS OF THE DEVICE

Power supply: 230 Vac 10%, 50/60 Hz

Max. power consumption: 1300W

Motors: 1/3 hp gas R404A5/8 hp gas R404A

Operating range: ambient to -68C

Precision: 1C

Dimensions (W x D x H): 600 x 700 x 1000 mm

Weight: 120 Kg

Working temperature: 0 to 50C

Storage temperature: -10 to 70C

Ambient relative humidity: lower than 90% rH not condensing

3. DEVICE PARTS

Graphic 13-2418A

Earth leakagecircuit breaker

Power switch Heating switch Temperature controller


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4. BRINGING INTO SERVICE

Place the apparatus to at least 50 cm from possible obstacles which you wall up, other

apparatuses, etc., in such way that the air scoop has a good circulation of air.

The cooling cryostat consists of an aluminum block and an air-cooled chiller.

The cryostat is protected against too high voltage by an earth leakage circuit breaker.

For safety reasons the earth leakage circuit breaker must be switched manually once aweek for checking its correct function.

Please before connecting to the mains make sure the voltage corresponds to the valueon the device's rear side.

Before switching on the device the first time the power switch and the earth leakage circuit breaker

are set to 0.

Switch on earth leakage circuit breaker: "I".

Switch on power switch.


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4.1. Preselection of the cooling temperature at the controller

To modify the temperature of job (set point) on the digital thermo regulator hold arrow down-

key. The display will show alternately the actual temperature and SP1. Now it is possible to

enter/modify set point value by pressing arrow-keys.

The value will be stored automatically after some seconds or press key P to confirm

immediately.

To this point follow the standard ASTM.

Press key HEATING to bring the apparatus to room temperature after a test.

It is not possible to control the heater by setting the temperature at temperature controller.

The device is always heated up to 25C.

This takes about 1h.

To re-cool the apparatus switch the heater off.

NOTE:

To heat the apparatus the main switch and heating switch must be in Position "I"!

Graphic 13-2418B

Earth leakage circuit breaker Power switch Heating switch Temperature controller


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5. SCOPE CAPP

Standard test method for pour point for use on any petroleum products (ASTM D 97) and only

petroleum products which are transparent in layers 40 mm. in thickness and with a cloud point

below 49C.

5.1. Accessories CAPP

16-0361 Test jar ASTM standard

16-0363 Insulating disks

16-0367 Distance ring (set of 10 pcs.)

16-0371 Thermometer ASTM 5C16-0375 Thermometer ASTM 6C

5.2. Spare Parts CAPP

Order of quantity

16-0361 Test jar ASTM standard 5

10-0493 Insulating disks 10

16-0367 Distance ring, set of 10 pcs. 1

16-0371 Thermometer ASTM 5C 1

16-0375 Thermometer ASTM 6C 1


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6. ASTMD97

6.1. Procedure

1. Pour the specimen into the test jar to the level mark. When necessary, heat the specimenin a water bath until it is just sufficiently fluid to pour into the test jar.

NOTEWhen the sample has been heated to a temperature higher than 45C during thepreceding 24 h or when the thermal history of the sample is not known, keep the sampleat room temperature for 24 h before testing it.

2. Close the test jar with the cork carrying the high-pour thermometer. See that thethermometer and the jar are coaxial, and the thermometer bulb is immersed so the

beginning of the capillary is 3 mm below the surface of the specimen.

If the expected Pour point is above +36C use a higher range thermometer such asIP63C or ASTM 61C.

Thermometer Temperature Range Thermometer Number

ASTM IP

High Cloud and Pour -38 to +50C 5C 1CLow Cloud and Pour -80 to +20C 6C 2CMelting Point +32 to +127C 61C 63C

3. For the measurement of pour point, subject the specimen in the test jar to the followingpreliminary treatment:

1. Samples having Pour Points above -33CHeat the specimen without stirring to 9C above the expected pour point, but to atleast 45C, in a bath maintained at 12C above the expected pour point, but at least48C. Transfer the test jar to a water bath maintained at 24C and commencesobservations for pour point.

2. Samples having Pour Points of -33C and belowHeat the specimen without stirring to 45C in a bath maintained at 48C and cool to15C in a water bath maintained at 6C. Remove the high cloud and pourthermometer and place the low cloud and pour thermometer in position.

4. Clean and dry the disk and the inside of the jacket to avoid frost formation which maycause erroneous results.Place the disk in the bottom of the jacket. Place the distance ring around the test jar25mm from the bottom. Insert the test jar with distance ring in the jacket.


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5. Begin to examine the appearance of the specimen when the temperature of thespecimen is 9C above the expected pour point (estimated as a multiple of 3C). At eachtest thermometer reading that is a multiple of 3C below the starting temperature removethe test jar from the jacket and remove condensed moisture with a clean cloth moistenedin alcohol (ethanol or methanol).

Tilt the jar just enough to ascertain whether there is a movement of the specimen in thetest jar. The complete operation of removal, wiping, and replacement shall require notmore than 3 s.Take great care not to disturb the mass of specimen nor permit the thermometer to shiftin the specimen; any disturbance of the spongy network of wax crystals will lead to lowand erroneous results.

If the specimen has not ceased to flow when its temperature has reached 27C, transfer

the test jar to the next lower temperature bath per the following schedule:

Bath Bath temperature setting (C) Sample temperature range (C)

1 0 1,5 Start to 92 -18 1,5 9 to 63 -33 1,5 -6 to 244 -51 1,5 -24 to 425 -69 1,5 -42 to -60

Table 1 Bath and sample temperature range

If the specimen in the jar does not flow when tilted, hold the jar in a horizontal position for

5 s and observe carefully. If the specimen shows any movement, replace the test jarimmediately in the jacket and repeat a test for flow at the next temperature, 3C lower.

6. If the specimen shows no movement when the test jar is held in a horizontal position for5s. Record the observed reading of the test thermometer.

NOTETo determine compliance with existing specifications having pour point limits attemperatures not divisible by 3C, it is acceptable practice to conduct the pour pointmeasurement according to the following schedule: Begin to examine the appearance ofthe specimen when the temperature of the specimen is 9C above the specification pourpoint. Continue observations at 3C intervals as described in 6 and 7 until thespecification temperature is reached. Report the sample as passing or failing thespecification limit.

7. For black specimen, cylinder stock and non-distillate fuel specimen, the result obtainedby the procedure described in 1 through 6 is the upper (maximum) pour point. If required,determine the lower (minimum) pour point by heating the sample while stirring, to 105C,pouring it into the jar, and determining the pour point as described in 4 through 6.


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6.2. Calculation and Report

Add 3C to the temperature recorded in 7. and report the result as the Pour Point, ASTM D

97. For black oil, etc., add 3C to the temperature recorded in 7. and report the result as

Upper Pour Point, ASTM D 97, or Lower Pour Point, ASTM D 97, as required.

6.3. Precision and Bias

Lubricating Oil and Distillate and Residual Fuel Oil.

Repeatability

The difference between successive test results, obtained by the same operator using the

same apparatus under constant operating conditions on identical test material, would in the

long run, in the normal and correct operation of this test method, exceed 6C for LubricatingOils and 3C for middle Distillate and Residual Fuels only in one case in twenty. Differences

greater than this should be considered suspect.

Reproducibility

The difference between two single and independent test results, obtained by different

operators working in different laboratories on identical test material, would in the long run, in

normal and correct operation of this test method, exceed 9C for Lubricating Oil and Distillate

and Residual Fuels only in one case in twenty. Differences greater than this should be

considered suspect.

Bias

There being no criteria for measuring bias in these test-product combinations, no statement

of bias can be made.


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7. ASTMD2500

7.1. Procedure

1. Bring the sample to a temperature at least 14C above the approximate cloud point.Remove any moisture present by a method such as filtration through dry lintels filterpaper until the oil is perfectly clear, but make such filtration at a temperature of at least14C above the approximate cloud point.

NOTEIn most cases of interference, filtration through dry lintels filter papers is sufficient. In thecase of diesel fuels, however, if the haze is very dense, a fresh portion of the sampleshould be dried by shaking 100 mL with 5 g of anhydrous sodium sulphate for at least 5min and then filtering through dry lintels filter paper. Given sufficient contact time, this

procedure will remove or sufficiently reduce the water haze so that the wax cloud can bereadily discerned. Drying and filtering should be done always at a temperature at least14C above the approximate cloud point but otherwise not in excess of 49C

2. Pour the sample into the test jar to the level mark.

3. Close the test jar tightly with the cork carrying the thermometer.The thermometer and the jar are coaxial, and the thermometer bulb is resting on thebottom of the jar.If the expected cloud point is above -36C use the High Cloud and Pour PointThermometer and the Low Cloud and Pour Point Thermometer if the expected cloudpoint is below -36C.

Thermometer Temperature Range Thermometer Number

ASTM IP

High Cloud and Pour -38 to +50C 5C 1CLow Cloud and Pour -80 to +20C 6C 2C

NOTEThermometers should be checked immediately prior to the test and used only if their icepoints are 0 1C, when the thermometer is immersed to the immersion line in an icebath, and when the emergent column temperature does not differ significantly from 21C.Alternatively, immerse the thermometer to a reading and correct for the resultant coolerstem temperature.

4. To avoid frost formation which may cause erroneous results see that the disk, distancering, and the inside of the jacket are clean and dry.

Place the disk in the bottom of the jacket. The use of a jacket cover while the emptyjacket is cooling is permitted.

Place the distance ring around the test jar, 25 mm from the bottom. Insert the test jar inthe jacket.

5. Maintain the temperature of the cooling bath at 0 1.5C.


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6. At each test thermometer reading that is a multiple of 1C, remove the test jar from thejacket quickly and without disturbing the oil, inspect for cloud, and replace in the jacket.This operation shall require not more than 3 s. If the oil does not show a cloud when ithas been cooled to 9C, transfer the test jar to a second bath maintained at atemperature of -18 1.5 C.

If the oil does not show a cloud when it has been cooled to-6C, transfer the test jar to a third bath maintained at a temperature of-33 1.5C. For the determination of very low cloud points additional baths are required,each bath to be maintained in accordance with the following schedule.

Bath Bath temperature setting (C) Sample temperature range (C)

1 0 1,5 Start to 92 -18 1,5 9 to 6

3 -33 1,5 -6 to 244 -51 1,5 -24 to 425 -69 1,5 -42 to -60

Table 1 Bath and sample temperature range

7. Report the cloud point, to the nearest 1C, at which any cloud is observed at the bottomof the test jar, which is confirmed by continued cooling.

NOTEA wax cloud or haze is always noted first at the bottom of the test jar where thetemperature is lowest. A slight haze throughout the entire sample, which slowly becomes

more apparent as the temperature is lowered, is usually due to traces of water in the oil.Generally this water haze will not interfere with the determination of the wax cloud point.Dry the sample as described in 1.


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7.2. Report

Report the temperature recorded in 7 as the Cloud Point, Test Method D 2500.


The precision of this test method as determined by statistical examination of inter-laboratory

results is as follows:

Repeatability

The difference between two test results, obtained by the same operator with the same

apparatus under constant operating conditions on identical test material, would in the long

run, in the normal and correct operation of this test method exceed 2C only in one case in

twenty.

Reproducibility

The difference between two single and independent results obtained by different operators

working in different laboratories on identical test material, would in the long run, in the normal

and correct operation of this test method, exceed 4C for distillate Fuels and lubricating Oils

and 3C for Biodiesel Products only in one case in twenty.

Bias

The procedure in this test method has no bias, because the value of cloud point can bedefined only in terms of a test method.


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8. SCOPE CFPP

This test method covers for the determination of the cold filter plugging point temperature of diesel

and domestic heating fuels.

8.1. Accessories CFPP

13-0422 Test jar 13-0445 Air Jacket nickel-plated brass

13-0424 Glass pipette with 20ml level 13-0446 Holding ring

13-0428 Sleeve for thermometer 13-0447 Stopper made of plastic

16-0371 Thermometer ASTM 5C/IP 1C 13-0444 Centering rack

16-0375 Thermometer ASTM 6C/IP 2C 13-0430 Filter apparatus complete

Graphic 13-0421A


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8.2. Spare Parts CFPP

13-0422 test jar

13-0424 glass pipette with 20ml level

13-0427 filter socket with sieve

16-0371 thermometer ASTM 5C

13-0428 sleeve for thermometer

13-0414 grip with cylinder inset

9. ASTMD6371

Graphics 13-0450C


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Prior to each test, the filtration unit in its individual parts, the test vessel, the pipette and the

thermometer must be washed with heptane.

Afterwards rinse with acetone and all parts are to be dried in a filtered airstream.

The cleaned and dried filtration unit is reassembled as shown in Illustration 13-0430A.

Fig. 13-0430A


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9.1. Procedure

1. A sample of 50 ml is filtered through a dry lint-free filter paper at room temperature(>15C). Establish the cooling bath temperature at -34 0.5C

2. Place the centering rack in the jacket.

3. The filtered sample is filled into the test jar up to the mark.The test jar is sealed with a stopper into which the glass pipette with the filtration unit andthe proper thermometer (see table) are inserted.The lower edge of filtration unit must remain on the bottom of the test jar - see illustration13-0421 A. The thermometer is not allowed to touch the wall of the test jar or the filtrationunit.

Expected CFPP Measuring range Thermometer

ASTM IPabove -30 C -38C to +50C 5C 1Cbelow -30C -80C to +20C 6C 2C

Do not change thermometers during the test. Adjust the apparatus in such a way that thebottom of the complete filter apparatus rests on the bottom of the test jar, and position thethermometer so that its lower end is 1.5 0.2 mm above the bottom of the test jar.

NOTEThe position of the lower end of the thermometer above the bottom of the test jar can beindirectly measured by marking the stem of the thermometer flush with the stopper when

the lower end of the thermometer is just touching the bottom of the test jar, and thenpulling the thermometer up such that the reference line is 1.5 0.2 mm above the top ofthe stopper.

4. Insert the test jar assembly in a vertical position into the jacket.

5. With the stopcock open to atmosphere; connect the glas pipette to the vacuum system bymeans of flexible tubing attached to the stopcock.

6. Switch on the vacuum unit.The U-tube manometer must indicate a vacuum of 2001 mm.

7. Start the test immediately, but if the cloud point of the sample is known, it is permitted towait until the specimen has cooled to a temperature of not less than 5C above its cloudpoint.

8. If the temperature of the sample has reached an suitable integer value, the three-waycock is set to connect the filtration unit with the vacuum system, and the timer is switchedon.This causes the sample to be drawn through the sieve of the filtration unit into the pipette.If the sample has reached the mark on the pipette, the three-way cock assumes itsoriginal position and the timer is stopped. Now the sample can flow back into the test jar

If the time required to reach the mark exceeds 60 s on the first attempt, the test

procedure is aborted and repeated with a new sample at a higher starting temperature.


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9. Test resultThe measurement is repeated for each of the sample's 1C drop in temperature. If thetemperature has been reached at which the pipette is not filled up to the mark within 60 s,the temperature at which the last filtration began is recorded as the CFPP. In case thepipette has not been filled within 60 s, yet upon opening the pipette via the three-waycock, the sample has not flowed back completely prior to the next intake cycle, thetemperature at the beginning of the last filtration is displayed as the CFPP.

10. In case the CFPP has not yet been reached when the sample temperature is -20C, thetest is to be continued in a second cooling bath in which the temperature is kept at aconstant -511C.For this the test jar with the filter unit is quickly transferred into a air jacket which is in thesecond cooling bath.

11. In case the CFPP has not been reached yet when the sample temperature is -35C, thetest is to be continued in a third cooling bath in which the temperature is kept at aconstant -672C.

12. In case no plugging of the filter occurs when the sample temperature is -51C, theprocedure is aborted. The result is recorded as "Not plugged at -51C".


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The precision of this procedure as determined by the statistical examination of the

interlaboratory test results is as follows:

Repeatability

The difference between results obtained on the same day by the same operator with the

same apparatus under constant operating conditions on identical test material, would in the

long run, with normal and correct operation of the test method, exceed 1.76C only in one

case in twenty.

Reproducibility

The difference between two single and independent results obtained by different operators

working in different laboratories on identical test material, would in the long run, in the normaland correct operation of the test method, exceed the values indicated by the formula:

0.102 (25-X) C

Where:

X is the average of the two results being compared, only in one case in twenty.

Bias

The procedure in this test method has no bias because the value of CFPP can be defined

only in terms of a test method.

Relative Bias

The current inter-laboratory tests confirm that there is no relative bias between the manual

and automated apparatuses. Both apparatuses are suitable for reference purposes.

Documents

Cloud and Pour