Aquamax KF

“ECO”

UK Distribution by: IMA Ltd, Parkwell House, Otley Road, Guiseley, West Yorkshire, LS20 8BH, England

Tel: +44(0)1943 878877 Email: [email protected] Website: www.ima.co.uk

Aquamax KF ECO v. 13.08

Aquamax KF ECO v.13.08

CONTENTS

Introduction …………………………………………………….……… Page 3

Principle of Measurement ……………………………………………… Page 4

Technical Specifications …..…………………………………………… Page 5

Unpacking & Parts List ……………………………………………… Page 6

Titration Cell Assembly Instructions …………………………………… Page 7-8

Filling & Changing Reagents ………………………………………….. Page 9

Front & Rear Panel Description ………..……………………………… Page 10

Setting Time & Date …………………………………………………… Page 11

Connection & Start Up Procedure ……………………………………… Page 12

Programming A Method ……………………………………………….. Page 13-18

Example Methods & Applications……………………………………… Page 19 - 21

How To Run A Test………………Examples V/SG & W/w…………… Page 22 - 23

Drift Compensation ……………………………….……………………. Page 24

Overtitration ……………………………………………………………. Page 24

Reagent Life ……………………………………………………………. Page 24

Cleaning the Glassware ………………………………………………… Page 25

Troubleshooting ……………………………………………………….. Page 26

Warranty ……………………………………………………………….. Page 26

Accessories ……………………………………………………………….. Page 27 - 29

2

Aquamax KF ECO v.13.08

G.R. Scientific Ltd.

Building 69

Wrest Park

Silsoe

Tel: +44 1525 404747 Fax: +44 1525 404848

E-mail: [email protected] Website: www.grscientific.com

Correspondence Address: Delivery Address:

Building 69

Wrest Park

Silsoe

Bedfordshire

MK45 4HS

Bedfordshire

MK45 4HS

United Kingdom United Kingdom

INTRODUCTION

Key personnel at G.R. Scientific are recognised experts in coulometric Karl Fischer titration technology and electrochemisty. They have designed and manufactured coulometric titrators since the early 1980’s and are widely regarded as some of the leading specialists in this technique.

The Aquamax KF ECO is an economical entry level titrator which has single injection port glassware, full numeric keypad for data entry, results manager software for data storage and retrieval. For use with generator electrodes either with or without frit. This small footprint unit offers excellent value.

Aquamax KF Formula reagents have been specially formulated for use with Aquamax KF titrators.

Formula A anode reagent is suitable for most routine applications and is especially useful for water content determination of oil samples, e.g. transformer oils, crude oils, etc. This anode reagent is supplied in “single shot” bottles of 100ml – No measuring of volumes required – No mixing of other solvents required. Cathode reagent Formula C is supplied in “single shot” 5ml vials which have “safety snappers” pre-fitted thereby reducing risk to the operator.

Where appropriate G.R. Scientific products include traceable calibration certificates and are backed up by a three year parts and labour warranty. These titrators are used by many leading companies in the oil, petrochemical, gas, pharmaceutical, biotechnology, automotive and power generation industries.

For a list of users, typical applications or details of our network of international distributors, please visit our website, www.grscientific.com , or contact G.R. Scientific Ltd. on:-

Tel: +44 1525 404747. Fax: +44 1525 404848. E-mail: [email protected]

To obtain the full benefits that this instrument can offer it is recommended that you read this user manual before assembling the unit.

Cou-Lo and Aquamax KF are registered trade marks of G.R. Scientific Ltd. “ACE” control system is patented technique owned by G.R. Scientific Ltd.

(All Aquamax KF power supplies are double insulated units that do not need an earth (ground) connection. These units are sealed and conform to CSA(LR84459), UL listings and CE requirements. Aquamax KF titrators only require a low voltage 15V input to the electronic / control circuitry. The moulded plastic casing of the instrument also provides additional insulation.)

3

Aquamax KF ECO v.13.08

PRINCIPLE OF MEASUREMENT

Karl Fischer titration is simply a means to measure water content of samples. Modern instruments, such as the Aquamax KF, use the coulometric principle, whereby the water present in the sample is coulometrically titrated to a predefined end point at which there is a minute excess of free iodine present.

Stoichiometrically, 1 mole of water will react with 1 mole of iodine, so that 1 milligram of water is equivalent to 10

⋅71 coulombs of electricity. Combining the coulometric technique with Karl Fischer titration, Aquamax KF titrators determine the water content of the sample by measuring the amount of electrolysis current necessary to produce the required iodine. This is an absolute technique which does not require calibration of the reagents. For further information, visit www.grscientific.com, and download the

PDF article titled “Recent Advances”.

SO

2

I

2

+SO

2

+3C

5

H

5

N+H

2

O

→ 2C

5

H

5

N.HI+C

5

H

5

N

O

SO

2

C

5

H

5

N +CH

3

OH

→ C

5

O

2I

 - 2e → I

SO

4

CH

3

H

5

N

H

2

Using the latest pulse current technology and our patented “ACE” control system, (Patent No.GB2370641), the Aquamax KF automatically selects the appropriate titration speed dependent upon the amount of water present in the sample. The titration speed is reduced as the end point is approached, and when the titration is completed the instrument prints out and displays the results. For a more detailed explanation of the technique, and a comparison with volumetric Karl Fischer titration, please visit our website, www.grscientific.com

4

Aquamax KF ECO v.13.08

Technical Specifications

Aquamax KF ECO

Titration Method:

Electrolysis Control:

Titration vessel:

End Point Detection:

End point indication:

Measuring range:

Moisture range:

Max. sensitivity:

Max. titration speed:

Max. current:

Drift compensation:

Precision:

Start delay time:

End delay time:

Calculation modes:

(user programmable)

Coulometric Karl Fischer titration

AC polarisation

0.1µg

400 ma

1ppm - 100% water

2.24 mg per minute

Automatically controlled

Weight/weight, (W/w)

0-30 minutes, user selectable

0-30 minutes, user selectable

Weight/dilution ratio, (W/K)

Patented “ACE” control system GB2370641

Visual display/print out/acoustic beep

Robust, single injection port glassware design

Possible: 1µg – 200 mg water. Typical: 1µg - 10mg water

10-100µg ± 3µg, 100µg-1mg ±3µg, above 1mg ±0.3%

Display format:

Method storage:

Volume/density, (V/SG)

Volume/volume, (V/v)

µg, mg/kg, ppm, %

Sample ID number:

Stirrer speed:

Languages:

Data outputs:

10 user programmable methods stored plus multi method via pc link

User programmable

Microprocessor controlled

Multi languages – user selectable

USB and RS232 ports

Removable Data storage: Flash drive (memory stick)

Data Entry: 15 key touchpad

Display:

Power supply:

Dimensions:

Weight:

40 character alphanumeric backlit LCD

250 x 245 x 120 mm

3.5kg

90-264V AC, 47-63 Hz. 12V DC car adapter/internal battery

5

Aquamax KF ECO v.13.08

UNPACKING & PARTS LIST

Inside the shipping carton you will find a plastic case which contains the glassware and accessories pack and the user manual. The Aquamax KF ECO titrator is located underneath the glassware case along with the mains power pack. Remove all of these items and check that they have arrived undamaged.

After unpacking your Aquamax KF ECO check that the glassware/accessories pack contains:-

Item

1 pce

Description

Titration Vessel single port

Single Port Cell

503047

1 pce

1 pce

1 pack

1 pce

Detector electrode

Generator electrode

PTFE sleeves (5 each size)

Desiccant tube & cap

503048

503049

503051

503058

1 pack

1 pce

1 pce

1 bottle

1 pce

1 pce

Injection septa (10)

1ml Gas Tight syringe

503059

503063

Luer needle Pair (17 & 19 gauge) 503067

Molecular sieve 503070

Stirrer bar

Funnel

503071

503072

ACCESSORIES

1 pce Mains power pack 401607

6

Aquamax KF ECO v.13.08

AQUAMAX KF TITRATION CELL

STEP BY STEP ASSEMBLY INSTRUCTIONS

Position titration vessel on Aquamax KF titrator

Place the PTFE sleevses on ground glass joints of each electrode.

Position electrodes on titration vessel. It is not necessary to overtighten these screw joints.

Connect leads to generator and detector electrodes then connect the leads to the titrator. Generator electrode lead connects to socket marked

“GENERATOR”

– detector electrode lead connects to socket marked

“DETECTOR”

Place stirrer bar inside titration vessel

Fit injection septa into plastic screw cap connectors and locate onto injection ports of titration vessel.

Fill drying tube with molecular sieve and locate on top of generator electrode

The assembled titration cell is now ready to be charged with reagents prior to use. Please be sure to assemble correctly every time the cell is cleaned or re-filled. It is recommended that the titrator is NOT switched on until after the titration vessel has been charged with reagents. This will avoid damage being caused to the electrodes by the stirrer bar. Avoid twisting the electrode leads otherwise they may become damaged.

7

AQUAMAX KF ECO TITRATION CELL

Aquamax KF ECO v.13.08

8

Aquamax KF ECO v.13.08

FILLING & CHANGING REAGENTS

The Aquamax KF ECO has been designed to operate with all major coulometric Karl Fischer reagents, however optimum performance can be obtained by using Aquamax KF Formula reagents which have been specifically formulated for use with these instruments. For most routine applications 100ml of Formula “A” (anode reagent) and 5ml of Formula “C” (cathode reagent) are used. When analysing Transformer oils, Crude oils and other petroleum products Formula “A” is especially suited as it contains other solvents to improve sample miscibility and solubility.

(When analysing samples of Ketones, amines or others which may interfere with the reaction it is advisable to use specialised reagents which can be obtained from various suppliers).

Although reagents can be poured into the titration vessel whilst it is located on the titrator, we recommend that the vessel and electrodes are removed from the instrument whilst this procedure is performed to avoid reagent spillage onto the instrument casing.

(Any spillage onto the instrument casing should be wiped off immediately to avoid damage or staining).

Remove the drying tube and injection septa. Using the funnel supplied, charge the titration vessel upto the lower line with

Formula “A” reagent. For your convenience these reagents are supplied in “single shot” bottles which contain 100ml so it is not necessary to measure any volumes – simply pour in the complete bottle

Also using the funnel, charge the inner chamber of the generator electrode with Formula “C” reagent which are supplied in “single shot” 5 ml vials which havce “safety snappers” pre-fitted thereby reducing risk to the operator.

(It is not necessary to clean the funnel between reagents.)

Reconnect the drying tube and injection septa so that the titration vessel is sealed from ingress of atmospheric moisture.

Locate the complete titration vessel onto the titrator and connect the electrode leads onto the appropriate sockets

The colours of anode and cathode reagent are only an illustration to show that there are two different liquids. These are not necessarily the exact colours of the reagents being used.

The Aquamax KF ECO titrator is now ready to be switched on.

Cathode Reagent Anode Reagent

9

Aquamax KF ECO v.13.08

DESCRIPTION

Front Panel

Keypad Display panel

Stirrer speed

Rear Panel

Power Jack:-

Fuse:-

RS232:-

USB-B:-

Nominal 18v DC 45w. Supply Input

3,15amp T type Time delay

Standard 4 wire RS232 Input / Output

Port.

Direct cable to PC / Results Manager

Port.

Removable Flash Memory Store Port. USB-A:-

RS232 Port. –

For updating titrator software, connecting to other equipment for remote controlling (software specific protocols to be provided).

USB-B Port. –

For connecting directly to PC to export data to Results Manager and enable results to be saved on files for future reference. (See Results Manager User Manual section)

USB-A Port. –

For exporting results data to a Removable Flash Drive (memory stick), when running sample tests in the field or remote locations, and subsequent transfer to PC at a later date for loading onto Results Manager files.

To use the memory store, insert Flash Drive into USB port A, titrator will see it and a symbol will appear on the display.

The symbol will appear blacked out while the drive is being written to and then as when idle.

The drive should only be removed when in the idle mode.

To read data saved on drive insert it into PC USB port. Start Results Manager, load selected file and then save in the format you require, see Results Manager user manual for full instructions.

10

SETTING THE DATE AND TIME

1. Switch on the Aquamax KF ECO and wait for it to display the following :

Aquamax KF ECO v.13.08

Aquamax KF ECO

Press START

2. Hold down the

START

KF ECO displays:-

Set Date / Time:

DD/MM/YYYY HH:MM:SS

3. Use the

•

decimal point key to move the cursor across the screen.

4. Use the numerical keys to set / alter the required number

START

key to save the changes and exit.

11

Aquamax KF ECO v.13.08

CONNECTION & START UP PROCEDURE

1. Assemble glassware (see Assembly Instructions

)

2. Charge vessel and generator electrode with reagents (see Filling & Changing Reagents

)

3. Locate assembled titration vessel onto the Aquamax

4. Connect electrode leads

5. Connect mains lead / power cord

6. Switch ON (using switch on rear panel) and wait for display to show:-

Aquamax KF ECO

Press START

(If required adjust the stirrer speed using the black toggle switch on the front of the instrument.)

microgram count

Aquamax xxxx

µg

|||||||||| 4 detector signal titration speed

At the end of the precondition period the display will show:-

Precondition

Dft = xxxx

µg

||| Drift Test

After the initial drift has been calculated, in micrograms of water per minute, the Aquamax KF is ready for operation.

Dft = xx xxxx

µg

|| 1 Ready

The background drift value will usually slowly decrease with time as the titration vessel becomes drier and more stable. Although it is possible for the titrator to be used at high drift values, it is advisable to wait until the drift value is below 20

µg/minute, and stable, before commencing, especially for low water content samples in the ppm ranges. The lower, and more stable the drift – the more accurate the result.

12

Aquamax KF ECO v.13.08

PROGRAM FUNCTIONS

When the Aquamax KF ECO displays Ready you can enter titration parameters, recall or edit existing methods, enter new method files, etc., by using the

PROGRAM, ENTER, CLEAR

and

•

keys.

Key Functions:-

PROGRAM

press PROGRAM key to scroll through menus listed.

ENTER

allows parameter values for the displayed menu to be entered into memory.

CLEAR

- this key has two functions:

(1) If you have finished entering data, press CLEAR and the Aquamax KF

Plus will return to the Ready condition.

(2) If you have started to enter an incorrect value, press CLEAR and the

Aquamax KF Plus will display the previously stored value, you can now select the correct value and press ENTER.

• ]

decimal point key allows scroll through of individual parameters in each menu.

When the required parameter is displayed, press ENTER to store it.

MENU LIST

Sample ID Number

Result Format

Calculation Mode

Start Delay Time

- upto 8 digits

-

µg, ppm, mg/kg or % water

- V/SG, W/W, W/K or V/v

- upto 30 minutes

Min. Titration Time - upto 30 minutes

End Sensitivity - 0 – 9 seconds

Beep Mode - off, keypress, end titration or both

Language - select language

Generator Electrode - with frit, without frit

Save Method - store upto 10 methods

See PROGRAMMING A METHOD for an explanation of each Menu List parameter

13

PROGRAMMING FLOW CHART

Aquamax KF ECO v.13.08

14

Aquamax KF ECO v.13.08

PROGRAMMING A METHOD

After the initial drift has been calculated, in micrograms (

µg) of water per minute, the Aquamax

KF

ECO

is ready for operation. It is now possible to step through the PROGRAM parameters and enter the required calculation data.

Dft = xx xxxx

µg

|| 1 Ready

The Flow Chart on the previous page may prove helpful. Press the PROGRAM key until the required option is displayed then simply follow the Flow Chart to enter the specific data values. Pressing

PROGRAM will move you on to the next prompt, pressing CLEAR will return to Ready condition. It is not necessary to step through all of the programme functions for every method, for example, if you only require to change the

Beep Mode from Off to Both – simple press PROGRAM until display shows Beep Mode, press the decimal point key

•

until display shows Both, then press ENTER and CLEAR to return to Ready.

SAMPLE ID NUMBER

Press PROGRAM → Display will show → Key upto 8 numbers → Press ENTER

PROGRAM

Sample ID No.

Sample ID No

12345678

ENTER

If you do not want to enter any further parameters simply press CLEAR to go back to the Ready condition.

Press PROGRAM if you want to continue entering other parameters

RESULT FORMAT

→

Display will show Press PROGRAM

PROGRAM

Result Format

µg

Results can be selected in

µg, ppm, mg/kg or % water.

If you want to select the format already stored in memory (and shown on display), press PROGRAM and the instrument will go to the next prompt. If you want to change format to give results in ppm, mg/kg or % you can scroll through these options by pressing decimal point key

•

until the required format is displayed, then press ENTER to store this in memory and PROGRAM to move onto the next prompt. If you have selected a result format in ppm, mg/kg or % the instrument will prompt you for the necessary calculation mode and data values.

Result Format

%

ENTER PROGRAM

Calculation Mode

V / SG

The display shows the calculated water content according to the programmed Result Format and

Calculation Mode program settings, ie. whatever has been chosen to be shown/printed at the end of the titration. The only exception to this is in the W/w mode when the Tare Weight has not yet been entered. In this case the display will show the

µg count. The PROGRAM key can be used to enter the Tare Weight at any time during the titration, once this has been done the display will start to show the calculated result in ppm, mg/kg or % water.

15

Aquamax KF ECO v.13.08

CALCULATION MODE

The Aquamax KF ECO has four standard calculation modes in memory. Each of these allow the instrument to divide the microgram count by the gram weight of sample introduced so that the calculated result can be printed out in either ppm or percentage of water.

Press the decimal point key

•

to scroll through the options available.

Select the calculation mode required and press ENTER.

The display will prompt you with the appropriate parameters.

Enter the numerical value for each parameter and press ENTER.

The four standard calculations are:-

1. Weight difference W/w

(This is the most accurate calculation and is suitable for almost all types of samples, powders,

liquids, gases, etc.)

Result (ppm or %) = microgram count

W - w

Where W = total weight of sampler + sample (gm)

w = tare weight of empty sampler (gm)

After entering the total weight (W) the instrument will return to the Ready condition. The Tare weight

(w) can be entered at any time during the titration by pressing PROGRAM, or at the end of titration. For ease of operation it is possible to enter the Total weight (W) as 0.0000gm, then place the full sampler on the balance and tare to zero. Thereafter it is only necessary to enter the weight difference (tare weight w) for each titration. This procedure reduces potential data entry errors.

2. Weight/Dilution ratio W/K

(Use this method if you need to dissolve a sample in another solvent. Suitable for samples which will not dissolve in the anode reagent or which might interfere with the KF reaction)

Result (ppm or %) = microgram count - bl

W where:

W = weight of sample dissolved (gm) x K

K = total volume of diluent + sample volume injected into Cou-Lo Aquamax e.g. bl = micrograms of water for same injected volume of diluent (

µg)

Accurately weigh approximately 2 gm of sample into a 20ml stoppered graduated flask. Make upto the volume line with suitable solvent / diluent. Using appropriate syringe inject 100

µl of diluted sample into the titration cell. Calculation parameters for this example would be:-

W

K bl

=

=

=

2 gm

20ml =

100

µl

200 microgram count of 100

µl injected volume diluent

16

Aquamax KF ECO v.13.08

3. Volume / Specific Gravity V/SG

(The most widely used technique for liquid samples. However, care must be taken to ensure

removal of all air bubbles from the syringe)

Result (ppm or % ) = microgram count

V x SG where V = volume of sample (ml)

SG = specific gravity

4. Volume V/v

Result % volume = microgram count

V x 1

⋅0 where V = volume of sample (ml)

This is essentially the same as V / SG mode, except that the sample S.G. is fixed at 1

⋅0

DELAY TIMES

The Aquamax KF ECO has been programmed to accept two different types of delay times, one at the start of titration and one at the end as a minimum titration time.

START DELAY TIME

The Aquamax KF ECO has a preset delay of five seconds which allows samples to be dispersed into the reagents before the titration starts. Some samples, particularly powders and viscous samples, may need additional time to fully dissolve. By selecting the start delay program, you can increase this time by upto 30 minutes.

Display shows: Start Delay Time

00 mins 00 secs

Select required time delay and press ENTER.

Whilst a delay time is in operation, the display will show “add sample” and the clock counter will show the time remaining before the start of titration. A start delay can be overridden by simply pressing START

MINIMUM TITRATION TIME

For some applications, such as certain gas samples or when using the Aquamax KF Plus combined with an oil evaporator or solids evaporator system it can prove useful to delay the end point of the titration. By selecting this parameter you can increase the minimum titration time by upto 30 minutes.

Display shows:

Min. Titration Time

00 mins 15 secs

Select required minimum time and press ENTER.

17

Aquamax KF ECO v.13.08

END SENSITIVITY

The sensitivity of detector signal as the end point is approached can be set from 0 – 9 seconds. The default value is 3 seconds and there are very few occasions when this may need to be altered. Decreasing this value can prove useful if samples cause interference, e.g. some Lube Oil samples.

BEEP MODE

Four options are available for the audible alarm (beeper) and they can be scrolled through using the decimal point key

•

until the required one is displayed. Then press ENTER.

The options are:

Off

Keypress

- beeper inactive

- beep once every time a key is pressed

End titration - beep three times at the end of a titration

Both - beep after every keypress and three times at the end of a titration

LANGUAGE

The Aquamax KF ECO can be programmed to show all display prompts and print outs in various languages. Use the decimal point key

•

to select language then press ENTER.

GENERATOR ELECTRODE

The Aquamax KF ECO can be operated using generator electrodes with or without frit (diaphragm). Use the decimal point key

•

to select either with or without frit then press ENTER. The titration electrolysis current settings are automatically adjusted for each style of generator and appropriate reagents.

SAVE METHOD

If you want to save a method for future use, this can be done by pressing a numerical key, 0 - 9, and

ENTER. All titration parameters, printer mode, beeper mode, etc. are stored automatically.

Display then shows:

Save Method

Done

Then press CLEAR and the instrument will revert back to the Ready condition.

RECALL METHOD

If any methods have been saved to memory then the first prompt (before Sample ID number) will be

“Recall Method”

When this prompt is displayed, simply press the number of the method file you wish to recall and press

ENTER. There are 10 method files available numbered from 0 to 9. The titration parameters etc will all be automatically recalled. Press PROGRAM to view the recalled method parameters or press CLEAR and the instrument will go back to the Ready condition.

If you do not want to recall a method, press PROGRAM to view the next prompt.

18

EXAMPLE APPLICATIONS

Raw Materials

Pharmaceutical

-

-

-

-

-

Inorganic and organic salts, oxides, peroxides and carbonates

Tablets

Salves and creams

Drugs

Vitamins

Cosmetics

-

-

-

Beverages

Dairy and Meat Products

Soaps, shower gels and shampoos

Dental Care and mouth rinse products

Sprays

Honey, Molasses and Sugars

Tobacco products

Animal Feed

Biological

-

-

-

-

Proteins and gelatins

Hormones and steroids

Dried plant material

Vaccines

Petrochem

-

-

-

-

Hydrocarbons

Lubricating, motor oil and greases

Hydraulic, insulating and transformer oils

Mineral oils

Plastics

Surfactants

Paints, lacquers and solvents

Leather, paper and textiles

Agriculture

Aquamax KF ECO v.13.08

19

Aquamax KF ECO v.13.08

EXAMPLE APPLICATIONS

LIQUID SAMPLES

Liquid samples are usually introduced into the titration vessel by using a syringe. The greater the amount of water introduced into the titration cell will cause the titration to take longer and also consume the reagents more quickly. It is recommended that the smallest representative amount of sample be used to ensure fastest titration speed and maximum sample throughput before reagents have to be replenished. Supplied as standard with every Aquamax KF titrator is a 1ml syringe and luer needle. These are suitable for injection of oil samples and water standards. Other volume syringes are commercially available from various suppliers. Please ensure that the needle is long enough to reach into the anode reagent.

This guide may be of assistance when selecting injection volume of samples:-

Expected water content…………….Suggested sample size

1 - 10 ppm……………… 1 or 2 ml

10 - 100 ppm……………… 1 or 2 ml

100 - 500 ppm……………… 0

⋅ 5 or 1 ml

500 - 1000 ppm……………… 0

⋅ 5 or 1 ml

0

⋅ 001 - 0 ⋅ 01 % ……………… 1 or 2 ml

0

⋅ 01 - 0 ⋅ 1 % ………..…..… 1 or 2 ml

0

⋅ 1

- 0

⋅ 5 % ……………… 0 ⋅ 5 or 1 ml

0

⋅ 5

- 1

⋅ 0 % ……………… 0 ⋅ 5 or 1 ml

1

⋅ 0

- 5

⋅ 0 % ……………… 0 ⋅ 2 ml above 5

⋅ 0 % ……………… 0 ⋅ 1 ml or less

Please note that these volumes are only a guide. You may wish to experiment with sample size to determine the optimum balance between repeatability, reagent depletion and speed of analysis.

CRUDE OILS

(IP 386 & 438, ASTM D1533, D4928, D6304, API MPMS Chapter 10.9, ISO 10337 & 12937)

Most coulometric reagents contain Methanol as the main solvent and as such it is possible that waxy deposits from crude oils can “drop out” and contaminate the electrodes, requiring more frequent and thorough cleaning of the glassware. This problem can be reduced by using Cou-Lo “Formula A” anode reagent which has been specially formulated for this application. The most common interference in crude oil samples is usually caused by mercaptans or sulphides. Samples containing alkyl groups will react stoichiometrically so that:

100 ppm Mercaptans would show as approximately 30 ppm water

100 ppm Sulphides would show as approximately 50 ppm water

In normal practice oils containing less than 500 ppm mercaptans or sulphides are regarded as having no appreciable effect. Repeatability problems are usually caused by sampling inaccuracies or improper homogenisation of the sample.

20

Aquamax KF ECO v.13.08

TRANSFORMER/INSULATING OILS

(ASTM D 1533, BS EN 60814, IEC 60814)

Due to the viscosity of these samples, and the fact that typical water content levels are in the range 5 – 40 ppm, it is usually necessary to inject sample volumes of 1 ml. This means that upto 50 samples would fill the titration cell. Provided that the other criteria governing reagent life, (total water titrated and reagent age), have not been reached, then it is possible to switch off the titrator and allow the oil to separate from the reagent. The oil can then be siphoned off and the instrument switched on again. After this operation it may take upto 30 minutes before the instrument settles down to a stable baseline. If it takes longer than 30 minutes then it is advisable to clean the cell and recharge with fresh reagents. For optimum performance use Aquamax KF “Formula A” reagent.

TURBINE / LUBRICATING OILS

For most Lube Oil applications a sample size of 1ml is sufficient. However, if it is suspected that the water content is above 1 %, then a sample size of 0

⋅ 2 to 0⋅ 5 ml is suggested.

KETONES AND AMINES

These can react with the Methanol present in most coulometric reagents resulting in inaccurate results and, in extreme conditions, titration end point being unattainable. For samples containing ketones, amines or aldehydes the use of specially formulated coulometric reagents for ketone samples is recommended.

POWDER SAMPLES

One of the main advantages of the coulometric technique is that reagents do not have to be replenished after every analysis, therefore the introduction into the titration cell of solid samples, which do not dissolve, is not recommended.

Three options available:-

• Powder samples which readily dissolve in the Anode reagent can be introduced using the optional powder sampler, part no. 503069. Calculation mode W/w.

• Powder samples which cannot be dissolved in the Anode reagent should be extracted or dissolved in a suitable solvent and then an aliquot injected. Calculation mode W/K.

Powder sampler

21

10.

11.

12.

6.

7.

8.

9.

1.

2.

3.

4.

5.

Aquamax KF ECO v.13.08

HOW TO RUN A TEST

Please read the section PROGRAMMING A METHOD then use the PROGRAMMING FLOW CHART before running any samples,

Example: Transformer oil sample by V/SG

Program the Aquamax KF ECO with parameters for the analysis. For Transformer Oil samples, these parameters are usually:-

Result Format

Calculation Mode

Sample Volume

= mg/kg or ppm

= V/SG

= 1.0 ml

= 0.875 Sample SG

Other parameters such as Sample ID number are optional.

ANALYSIS METHOD

Confirm that Aquamax KF ECO is in “Ready” mode

Flush 1.0ml syringe several times (minimum 6 times) with sample

Fit luer needle and flush through with sample

Draw sample into syringe beyond the 1.0ml marking

Invert syringe so that any air bubbles can be ejected through the needle and adjust syringe plunger to the 1.0 ml mark

Wipe off excess sample from outside of needle using a clean, dry tissue or paper towel

Pierce needle through injection septa of titration vessel (1 – 2 cm)

Press START

Push needle into anode reagent and inject sample

Withdraw needle from titration vessel

Read result, in mg/kg (ppm) water, on display and printout

Repeat steps 2 – 11 if duplicate result required

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Aquamax KF ECO v.13.08

Example: Powder sample by W/w

Program the Aquamax KF ECO with parameters for the analysis.

ANALYSIS METHOD (1)

1. Confirm that Aquamax KF ECO is in “Ready” mode

2. Place a suitable amount of sample in the powder sampler (p.n. 503069) and seal with stopper provided.

3. Weigh sampler

4. Press PROGRAM until Calculation Mode displayed then select W/w

5. Enter the sampler weight when prompted by display, then press ENTER / CLEAR

6. Remove the injection septa port, press START, and pour the sample inside the titration vessel ensuring that sample does not stick to the inside of the vessel wall.

7. Reweigh the sampler.

8. The net weight of sampler can be entered either during the titration by pressing PROGRAM or waiting until the end of titration when display will prompt TARE Weight. Enter the weight then press CLEAR.

ANALYSIS METHOD (2)

1. Confirm that Aquamax KF ECO is in “Ready” mode

2. Place a suitable amount of sample in the powder sampler (p.n. 503069) and seal with stopper provided.

3. Place sampler on balance and tare to zero

4. Press PROGRAM until Calc. Mode displayed then select W/w

5. Enter the sample weight as 0.0 gram, then press ENTER / CLEAR

6. Remove the injection septa port, press START, and pour the sample inside the titration vessel ensuring that sample does not stick to the inside of the vessel wall.

7. Reweigh the sampler.

8. The weight difference of sampler can be entered either during the titration by pressing PROGRAM or waiting until the end of titration when display will prompt TARE Weight. Enter the weight then press

CLEAR.

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Aquamax KF ECO v.13.08

DRIFT RATE COMPENSATION

At the start of any titration, the drift value in the top left corner of the screen (in micrograms per minute), is stored in memory. This ensures that the displayed result is corrected for any ingress of atmospheric moisture during the titration period.

Whilst in READY condition, the Aquamax KF ECO continually compensates for any drift caused by atmospheric moisture ingress or reagent decomposition and displays this information, which is updated every 10 seconds. If the drift value is above 25 μg /minute the display will show High Drift **XX**. This is a warning that the value is high, however the instrument can still be used by simply pressing START to continue. Provided the drift rate is stable then it usually acceptable to continue operation. The Aquamax titration cell design can provide drift val ues down to less than 5 μg /minute but can also operate at much higher values. The maximum drift value is 60 μg /minute but we recommend operating upto a maximum of

25 whenever possible.

If the drift value is above 60

µg per minute the display will read

“EXCESS DRIFT - SEE INSTRUCTION MANUAL”

Most common causes of excess drift are:

Titration vessel not properly sealed (check septa & fittings).

Reagent almost depleted (clean & recharge the cell).

Sample introduced before pressing START key.

Trace moisture on cell walls.

If excess drift occurs, switch the instrument off, remove titration cell from clamp, gently swirl the anode reagent around the cell walls, replace cell in clamp, switch instrument on and allow to precondition.

OVERTITRATION

If the detector electrode senses too much Iodine in the titration cell, usually caused by instrument being left unoperated for a long period, the display will read :-

“OVERTITRATION - SEE INSTRUCTION MANUAL”

Simply add 3 - 5 microlitres of water, or a small amount of a known wet sample, until the detector signal bars on bottom left of display are activated. Then instrument will automatically carry out its precondition.

REAGENT LIFE

There are three main factors which govern the life of reagents, and therefore, the frequency of cleaning and recharging the titration cell:

1. The physical size of the titration cell allows for 50 – 60 mls of sample to be added. For the analysis

2. of most liquid samples (e.g. solvents) the Aquamax KF ECO normally only requires a few microlitres to be injected, therefore the maximum volume of 50 – 60 mls should not become a limiting factor. (Oil samples are an exception and are dealt with elsewhere in this manual).

The total amount of water that can be analysed before saturation of the reagents varies slightly from one reagent manufacturer to another. Typically a 100 ml charge of Anode reagent (Formula

“A”) will analyse upto 1 gm water, whilst a 5 ml charge of Cathode reagent (Formula “C”) will

3. analyse upto 250 mg water. Considering that the injected sample volume is normally small, and also that the analysis is usually for the determination of low levels of water, these water capacity values are not normally a limiting factor.

Similar to all other Karl Fischer reagents, coulometric reagents will deteriorate when exposed to sunlight and with increases in temperature. Placing the instrument in direct sunlight or near to a heat duct can decrease the reagent life. As reagents age, the titration speed will reduce and the drift value will increase.

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Aquamax KF ECO v.13.08

CLEANING GLASSWARE

IMPORTANT

The platinum mesh and wires of the electrodes are fragile and can be easily bent or broken. Extreme care

MUST be taken when disassembling, cleaning and reassembling the titration cell. The generator electrode

is the most expensive part of the Aquamax KF glassware. DO NOT USE BRUSH TO CLEAN INSIDE

ELECTRODE AS THIS COULD DAMAGE CONNECTIONS. Coulometric reagents are flammable

and toxic, so care should always be taken when handling them and when cleaning the glassware. Whenever possible this should be done in a safe area, e.g. inside a fume cupboard. Reagents should not be recharged while the titration cell is still attached to the titrator. See page 11 on charging procedure.

Under normal circumstances the titration cell can be used for a large number of samples before having to replenish the reagents. Once the reagents have been exhausted, or when the titration cell maximum volume has been reached, it should simply be necessary to:-

1.

2.

3.

4.

DISASSEMBLE titration cell (disconnect leads from titrator)

EMPTY the titration cell and generator electrode

RINSE all parts with methanol. Do not use brush on electrodes.

DRY all parts

5.

6.

REASSEMBLE glassware

RECHARGE with fresh reagents

If the cell is heavily contaminated then it may be necessary to clean it more thoroughly. For oil samples, cleaning with chloroform or xylene is suggested, whilst for salt deposits a water wash may be required. Use whichever solvent is most suited for the sample type. The titration vessel can even be cleaned with hot soapy water and a bottle-brush. However, after cleaning with suitable solvent, all glassware parts, MUST be rinsed inside and out with methanol. They can then be dried with a warm air blower, such as a domestic hair dryer, placed in a low temperature oven at 40 – 50

° C, or left in a desiccator.

After being fully dried, reassemble the titration cell and charge with fresh reagents.

THE MORE THOROUGHLY THAT THE TITRATION CELL IS CLEANED AND DRIED, THE

FASTER THE INSTRUMENT WILL STABILISE READY FOR OPERATION AFTER

RECHARGING REAGENTS.

Under normal conditions, the Aquamax KF

ECO

should be ready for operation within 5 – 10 minutes after reassembly, however it could take up to 20 minutes before to completely stabilise if the drying procedure has not been properly carried out.

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Aquamax KF ECO v.13.08

TROUBLESHOOTING

OVERTITRATION

Detector senses too much Iodine. Usually caused by old reagents or stirrer switched off. Check stirrer speed. Add 3-5 microlitres of water until detector bars activate, and allow to precondition.

EXCESS DRIFT

Indicates excess moisture ingress or condensation on cell walls. Switch OFF. Remove titration cell from clamp and gently swirl anode reagent around the cell walls. Reconnect, switch ON, and allow to Precondition.

LONG PRECONDITIONING TIME

Normally caused by glassware not being sufficiently dried before assembly. Re-clean glassware and electrodes, dry thoroughly and charge with fresh reagents.

PROGRESSIVELY LOWER RESULTS FOR SAME SAMPLE

Moisture contamination of syringe. Flush syringe and needle with sample several times before beginning new test.

POOR REPEATABILITY FOR SAME SAMPLE

Sample size probably too small or moisture contamination of syringe. Increase sample size and flush syringe and needle several times before beginning new test.

Call G.R. Scientific Ltd or your local dealer for suggestions on sampling technique for your application.

E-mail: [email protected]

TEL: +44 1525 404747 FAX: +44 1525 404848

INSTRUMENT CARE

Although the instrument casing is highly resistive to most solvents care should be taken to ensure that any spillage is wiped off immediately to avoid staining or possible damage to the paint surface.

WARRANTY

Under the conditions of our warranty, all faults which are proved to be due to material, construction or manufacturing defects, which occur within 36 months of the delivery date, will be repaired or replaced, (at our discretion), free of charge at our premises. Freight costs will be chargeable along with any inspection work which was not necessitated by manufacturing or material defects. Breakages of glassware or electrodes are not covered by this guarantee. In the event of instrument failure during the warranty period, written authorisation must be obtained from the manufacturer prior to shipping.

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Aquamax KF ECO v.13.08

OTHER PRODUCTS IN THE GR SCIENTIFIC RANGE

Aquamax KF

Plus

This is the truly versatile model which includes a built-in battery and printer to enable use in areas where the power supply is irregular. Low Drift Cell twin port glassware, results manager software and accessories are supplied as standard. As well as being a stand-alone instrument, the Aquamax KF Plus can be combined with our Oil Evaporator, and soon a new Solids

Evaporator system. Suitable for a wide range of applications the

Aquamax KF Plus can be used to determine water contents of liquids, gases and solids

.

Aquamax KF

Portable

Designed primarily for the oil and power industries, this titrator is the only model on the market with a carry handle attached directly to the unit. It also features a protective stainless steel cage, built-in printer and single button operation for water standards analysis, using either distilled water or water pellets. Specially designed

Low Drift Cell twin port glassware avoids the need for PTFE sleeves or grease on the electrodes to seal titration cell from moisture invasion.

Aquamax KF

OPS Workstation

Also available is a carry case for transportation in the field and an

OPS Workstation which includes everything the user needs, such as syringes, standards, reagents, etc. all in one footprint for ultimate efficiency.

Aquamax KF

Oil Evaporator

For combined operation with the Aquamax KF Plus titrator to determine water content of additives, lube oils, base oils, automatic transmission fluids, hydrocarbon solvents, and other petroleum products.

Aquamax KF

Solids Evaporator

For combined operation with the Aquamax KF Plus titrator to determine water content of solids such as plastics, nylons, paper, powders, etc.

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Aquamax KF ECO v.13.08

Aquamax KF

Volumetric

An adaptable titrator capable of titrating with superior accuracy and precision even for samples with low moisture content. Dual syringes enable the operator to dispense titrant and standard automatically eliminating cell opening which may introduce moisture to the system. The Aquamax KF Volumetric comes equipped with a solvent handling system to reduce cell conditioning time and can be connected directly to your laboratory balance via serial interface. Choose from four pre-programmed methods or develop a custom method for almost any application or sample type.

microTAN

Titrator

An innovative micro system for measuring Total Acid Number which enables the user to save up to 75% of organic solvent per sample analysis compared to standard potentiometers.

Supplied with an optimized titration vessel and micro combination electrode that regenerates to optimum efficiency in minutes and offers excellent stability for non-aqueous titrations.

microTAN

OPS Workstation

Everything you need in one footprint and transportable! The

MicroTAN workstation is an organised workspace containing all equipment and chemicals required to run your samples.

MicroTAN unit, chemicals and accessories are contained in a sturdy outer case with a firm foam lining in an ergonomic arrangement. Optional accessories include a bottle top dispenser for dedicated dispensing of titration solvent and a mini thermal printer.

TitraMax

Titrator

Is a simple, versatile yet robust potentiometer for measuring TAN,

TBN, mercaptan sulphur and analysis of petroleum products. Preprogrammed methods that conform to ASTM standards and an interchangeable burette system with intelligent volume recognition are key features of the Titramax. In addition each unit is supplied with bespoke UK manufactured electrodes for optimum performance and reproducible results.

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Aquamax KF ECO v.13.08

E-chem

pH & Conductivity meters

The E-chem range of pH/conductivity benchtop meters have been developed to provide cost effective, robust and simple to use solutions for your needs. The E512 pH meter offers research grade specifications with a comprehensive range of features and functions, ideal for general laboratory, QC and GLP based applications. Producing rapid and reliable results that are accurate and reproducible, are paramount in all field and laboratory environments. All products within the E-chem series cover a wide range of applications in areas including, food and beverage, water, environmental, power and petrochemical industries

E-chem

electrodes, buffers, standards

We offer a range of combined pH, glass, epoxy tough and reference electrodes for every application and budget. All of our electrodes are manufactured in the UK so you are guaranteed. Uncompromised quality and fast delivery

For accurate pH and conductivity measurements, we offer certified standards traceable to NIST and are tested using ISO 17025 accredited method. Our conductivity standards have an accuracy of ±1.0% and their shelf life is valid regardless of when the bottle was first opened, provided good laboratory practice is adhered to. Our pH Buffers are manufactured to exacting specifications according to NIST with an extended shelf life. Temperature dependence data is printed on the labels as are lot numbers and expiry dates.

GR Scientific Service

We want you to maximise the return on your equipment through a service program tailored to your requirements from when you purchase our equipment which includes:

- Support and repair

- Maintenance and calibration

- Training and installation

- Quality assurance and certification

Our dedicated service staff are on hand to help in the unlikely event that your equipment develops a fault.

Please contact us using the details provided below to discuss the next step.

For further information about any of our products, pricing or details about local representatives, just contact

Telephone: +44 (0) 1525 404747 Fax: +44 (0) 1525 404848

Email: [email protected] Web: www.grscientific.com

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