Hach APA 6000 Operation Manual

Catalog Number 62000-18

APA 6000™ High Range Hardness Process Analyzer

Operation Manual

© Hach Company, 2002, 2005. All rights reserved. Printed in the U.S.A.

eac April 2005, Edition 2

Table of Contents

Safety Precautions.................................................................................................................................................... 3

Specifications............................................................................................................................................................ 4

Section 1 Instrument Overview........................................................................................................................ 7

1.1 How to Use the Manuals..................................................................................................................................... 7

1.2 General Description ............................................................. ... .... ... ... ... ............................................................... 7

1.2.1 Instrument Enclosure............................................ ................................................ ... .... .. ............................ 7

1.2.2 Autoburette Module ....... ... ... ................................................. ... ... .... ... ........................................................ 7

1.2.3 Colorimeter Module, Holding Coil, and Reaction Coil ............................................................................... 8

1.2.4 Rotary Valve Module ........ ... .... ... ................................................ .... ... ... ... .................................................. 8

1.2.5 Mixer Module........................................... ... ... ... .... ... ................................................ .................................. 8

1.2.6 Plumbing Diagram and Tubing Lengths.......................................... ........................................................... 8

1.2.7 Vortex Sample Conditioning Block........................................................................................................... 11

1.2.8 High Range Hardness Reagents............................................................................................................. 11

Section 2 Theory of Operation........................................................................................................................ 13

2.1 Method of Analysis...................................................................................... ... ... ... .... ......................................... 13

2.2 Reagent Consumption ...................................................................................................... ................................ 14

Section 3 Sequence of Instrument Events.................................................................................................. 15

Section 4 Parameter Specific Functions...................................................................................................... 22

4.1 Calibration History................................... ................................................. ... ... ... ... ............................................. 22

4.2 Measurement Options............................. ... ................................................. ... ... ................................................ 22

Section 5 Bench Method Procedure.............................................................................................................. 23

5.1 Standardization................................. ................................................ ... .... ... ... ................................................... 23

5.2 Standardization Procedure ..................... ... .... ... ................................................ ... .... ... ... ................................... 23

5.3 Testing Samples for Total Hardness.................................................................................................................. 24

5.3.1 Total Hardness Digital Titrator

5.3.2 Total Hardness Buret Method.................................................................................................................. 26

®

Method.................................................................................................. 25

Section 6 Replacement Parts.......................................................................................................................... 27

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Table of Contents

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Safety Precautions

6200018safety.fm Safety Precautions

Page 3

Specifications

Performance

Specifications are subject to change without notice.
See instrument-specific specifications in the APA 6000™ Process Analyzer

Manual, Cat. No. 62005-18.

Sample Requirements

Range:10 to 1000 mg/L as CaCO

Note: If sample is outside the specified instrument range, a sample out error

may occur.

Accuracy: ±5% of reading or ±2 mg/L as CaCO3, whichever is greater
Repeatability: ±5% of reading or ±2 mg/L as CaCO
Response Time: For single channel instruments, less than 17 minutes for

90% response to step change at sample inlet

Cycle Time: 8.2 minutes (average)
Sample Temperature Range: 5 to 50 °C (41 to 122 °F)
Operating Temperature: 5 to 50 °C (41 to 122 °F)
Relative Humidity: 5 to 95% relative humidity, non-condensing

Sample Pressure: 0.5 to 30.0 psig (0.03 to 2.04 bar)
Sample Temperature: 5 to 50 °C (41 to 122 °F)

3

, whichever is greater

3

Page 4

Specifications

Sample Flow: 100 to 2000 mL/min. maximum
Sample Inputs: Up to two sample streams

6200018Specs.fm

Operation

DANGER

Handling chemical samples, standards, and reagents can be dangerous. Review the necessary Material
Safety Data Sheets and become fami liar with all safety proced ures before handling any c hemicals.

DANGER

La manipulation des échantillons chimiques, étalons et réactifs peut être dangereuse. Lire les Fiches de
Données de Sécurité des Produits (FDSP) et se familia ris er avec toutes les procédures de sécurité avant
de manipuler tous les produits chimiques.

PELIGRO

La manipulación de muestras químicas, estándares y reactivos puede ser peligrosa. Revise las fichas
de seguridad de materiales y familiarícese con los procedimientos de seguridad antes de manipular
productos químicos.

GEFAHR

Das Arbeiten mit chemischen Pr oben, Standar ds und Reagenzien ist mit Gef ahren verbund en. Es wird de m
Benutzer dieser Produkte empfohle n, sich v or der Arbeit mit sicheren Verfahrensweisen und dem ric htigen
Gebrauch der Chemikalien vertraut zu machen und alle entsprechenden Materialsicherheitsdatenblätter
aufmerksam zu lesen.

La manipolazione di campioni, standard e reat tivi chimici può esse re pericolosa. La preghiamo di prendere
conoscenza delle Schede Techniche necessarie legate alla Sicurezza dei Materiali e di abituarsi con tutte
le procedure di sicurezza prima di manipolare ogni prodotto chimico.

6200018operation_stop.fm Operation

PERICOLO

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Section 1 Instrument Overview

1.1 How to Use the Manuals

This instrument requires two manuals for complete operating instructions.
The APA 6000™ Installation and Maintenance Manual (Cat. No. 62005-18)
provides instructions for instrument installation, menu setup, operation,
maintenance, and troubleshooting.

This Paramet er-specific Operation Manual (Cat. No. 62000-18) contains
information related to parameter specific instrument components and
software functions. Descriptions of rea gents and standards and their
consumption rates, method of analysis, operational sequence, and bench
comparison testing are all addresse d in this paramete r spec ific ma nual.

1.2 General Description

The APA 6000™ High Range Har dness Process Analyzer is a
microprocessor-controlled process analyzer designed to contin uously monitor
a sample water stream for total hardness (calcium, magnesium, and heavy
metals). Typical samples ma y include drinking w ater , r aw w ater , cooling w ater ,
and industrial water.

The analyzer can measure one or two sample streams with a cycle time of

8.2 minutes. It uses a colorimetric chemical method to determine hardness
concentrations in the sample stream. Measurement unit options include ppm,
mg/L, g/gal, and Gdh (German degrees of hardness).

1.2.1 Instrument Enclosure

Data communication and retrieval is done via the AquaTrend
keypad and display.

The reagent containers are sized to provide approximately 30 days of
continuous operation. The reagents are factory-filled in one-liter containers
and meet Hach quality standards. Prepare Reagent 2 prior to use by mixing
one bottle of Indicator Powder (Cat. No. 27931-35) into 1 liter of Buffer
Solution (Cat. No. 27930-53). Both powder and solution are included in the
Reagent 2 Kit (Cat. No. 27936-00).

The instrument enclosure houses various modules, the instrument’s
power supply and control circuitry. Within the enclosure, a module panel
separates sensitive electrical components from the wetted parts.
All openings to the module panel are gasketed to protect against leakage.
The module panel folds out t o allow acce ss to the electrical connections at t he
back of the instrument.

The internal instrument temperature is factory set at 50 °C (120 °F). The
design of the analyzer door and instrument panel provides a small, insulated
space ensuring temperature control for accurate analysis. In order for the
temperature control system to functio n pr op e rly, the instrument door must
remain closed and latched during operation.

®

Interface

1.2.2 Autoburette Module

6200018overview.fm Instrument Overview

The analyzer uses a positive-displacement autoburette to measure and
move fluids through the various analytical components in the instrument.
The autoburette module consists of a clear acrylic block which houses a
ceramic piston, a double seal for the piston, a linear actuator, a two-way
solenoid valve, and control circuitry. The overall volume of the burette is

Page 7

Section 1

1.6 mL and it can move in either direction to aspirate o r dispense f luids o v er a

0.1 to 8.0 mL/minute range.

1.2.3 Colorimeter Module, Holding Coil, and Reaction Coil

Samples are measured in a temperature-controlled single-wavelength flow
cell. Light from an LED in the colorimeter passes t hrough a 6 00 nm ba ndpass
filter. The path length is 8.75 mm (0.344 inches). The temperature is
controlled at 50 °C (120 °F).

The holding coil is a length of 0.030 inch ID Tefzel tubing arranged to minimize
mixing. The holding coil allows low volumes of representative sample to be
measured each cycle. The holding coil also effectively brings the sample and
reagents to the temperature control point. Without the holding coil, “old”
sample would need to be flushed from the b ure tte. This would require at least
10x greater volume and longer analysis times, higher wastes, more sample
conditioning, more standard consumption, etc.

This parameter also utilizes a 550 µL reaction coil. The reaction coil allows
reproducible dispersion (or spreading) of the sample/indicator with the titrant
(acid). As the two fluids disperse, a full ran ge of concentrations result. This
range begins with all sample/indicator then transitions to a greater
concentration of titrant. Eventually, a maximum concentration of titrant is
reached and as the transition continues, the titrant strength drops until only
sample/indicator is present again. The reaction coil is placed between the
valve and d etector . After the dispersion described abov e occurs , the response
is measured as fluids pass through the detector.

1.2.4 Rotary Valve Module

The rotary valve directs fluids to various components in the instrument. The
valve is a selection valve with a common port at the center. An internal rotor
turns to align a grove between the center port and any one of the ten a va ilable
ports around the perimeter. The valve has a face sealing design. All tubing is
factory-assembled and labeled for each individual chemistry.

1.2.5 Mixer Module

The mixer module mixes reagents with the sample or standards. Fluid
normally enters and exits through the bottom of the module. The openings at
the top supply an overflow and vent. The vent line is connected to the drain
block. The mix er is made of acrylic and has an appro ximate v olume of 2.0 mL.
The mixer is filled, emptied, and rinsed during a typical measurement cycle.
Mixing and excess air removal is accomplished via a magnetic stir bar.

1.2.6 Plumbing Diagram and Tubing Lengths

Figure 1 on page 10 shows the user-replaceable tubing on the analyze r and
Table 1 on page 10 describes the terminal end size of each tube. The tubing

is 0.030 inch ID Tefze l. The small diameter allows for low-volume and high­flow rates. A higher fl ow rate , along with properly applied sample conditionin g,
prevents the tubing from plugging.

General information for replacing the tubing is presented in the APA 6000
Installation and Maintenance Manual (Cat. No. 62005-18).

Page 8

General Description

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Section 1

CAUTION
To familiarize yourself with
handling precautions, dangers
and emergency procedures,
always review the Material Safety
Data Sheets prior to handling
containers, reservoirs, and
delivery systems that contain
chemical reagents and standards.
Protective eye wear is always
recommended when contact with
chemicals is possible.

PRUDENCE
Pour se familiariser avec les précautions à prendre lors de la manipulation, les
dangers et les procédures d'urgence, to ujours lire les Fiches de Données de
Sécurité des Produits avant de manipuler les récipients, les réservoirs et les
systèmes de distribution contenant les réactifs chimiques et les solutions
étalons. Il est toujours recommandé de porter des lunettes de protection
lorsqu'un contact avec les produits chimiques est possible.

CUIDADO
Para familiarizarse con las precauciones de manipulación, los peligros y los
procedimientos de emergencia, siempre estudie las Hojas de Datos de
Seguridad de los Materiales antes de manipular recipientes, depósitos y
sistemas de entrega que contengan reactivos y patrones químicos. Siempre se
recomienda el uso de protectores oculares cuando sea posible el contacto con
productos químicos.

VORISCHT
Es wird dringend empfohlen, die Sicherheitsdatenblätter vor der Handhabung
von Behältern, Tanks und Zufuhrsystemen, die chemische Reagenzien und
Standardsubstanzen enthalten, aufmerksam durchzulesen, damit Sie sich mit
den beim Umgang mit diesen Chemikalien no twendigen Vorsichtsmaßnahmen,
Risiken und Notfallschutzmaßnahmen vertraut machen. Es wird empfohlen, in
allen Situationen, in denen mit einem Kontakt mit Chemikalien zu rechnen ist,
eine Schutzbrille zu tragen.

ATTENZIONE
Per familiarizzare con misure di precauzione di controllo manuale, con
procedure pericolose e di emergenza, rileggere sempre le schede di sicurezza
del materiale prima di maneggiare contenitori, imballaggi per spedizione che
contengono reagenti chimici e standards. Si consiglia di indossare sempre gli
occhiali protettivi quando è possibile un contatto con agenti chimici.

6200018overview.fm General Description

Page 9

Section 1

Figure 1 Plumbing Diagram for a High Range Hardness Analyzer

Table 1 Replacement Tubing Lengths for Figure 1

Item Description Length From... To...

1 Reaction coil - part of Temperature Control Block Call Service Port 1 Reaction coil
2 Tefzel tubing, 0.03 ID x 0.062 OD 60 cm (24 in.) Port 2 Sample 1
3 Blank port — — —
4 Tefzel tubing, 0.03 ID x 0.062 OD 145 cm (57 in.) Port 4 Standard 1
5 Tefzel tubing, 0.03 ID x 0.062 OD 152.5 cm (60 in.) Port 5 Standard 2
6 Tefzel tubing, 0.03 ID x 0.062 OD 87.5 cm (34.5 in.) Port 6 Waste
7 Tefzel tubing, 0.03 ID x 0.062 OD 152.5 cm (60 in.) Port 7 Reagent 3
8 Tefzel tubing, 0.03 ID x 0.062 OD 152.5 cm (60 in.) Port 8 Reagent 2

9 Tefzel tubing, 0.03 ID x 0.062 OD 145 cm (57 in.) Port 9 Reagent 1
10 Tefzel tubing, 0.03 ID x 0.062 OD 19 cm (7.5 in.) Port 10 Mixer in
11 Tefzel tubing, 0.03 ID x 0.062 OD 70 cm (27.5 in.) Mixer module out Mixer drain
12 Tefzel tubing, 0.03 ID x 0.062 OD 17.5 cm (7 in.) Two-way NC Wash solution
13 Tefzel tubing, 0.03 ID x 0.062 OD 16 cm (6.3 in.) Two-way out Autoburette bottom
14 Tefzel tubing, 0.03 ID x 0.062 OD 30.5 cm (12 in.) Seal wash bottom Autoburette top
15 Tefzel tubing, 0.03 ID x 0.062 OD Call Service Reaction coil Colorimeter in
16 Holding coil Call Service Colorimeter out Drain
17 Common port line 17 cm (6.7 in.) Center port Holding coil

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General Description

6200018overview.fm

1.2.7 Vortex Sample Conditioning Block

The sample conditioning bloc k consists of a 0.5 µm ceramic filter held within a
flow block. Unfiltered sample flows around the outside of the filter and serves
to continuously self-clean the filter elemen t. Sample is dra wn through the filter
on demand. Regular maintenance of the sample conditioning is required for
proper operation.

1.2.8 High Range Hardness Reagents

The APA 6000™ High Range Hardness Process analyzer uses six reagents.
Each is supplied in a 1-L bottle designed to provide reagents for 30 days of
continuous use.

• Reagent 1 is a masking solution that adjusts the pH of the sample.

• Reagent 2 is an indicator u sed t o dete rmine the endpoints of t he titration.

It is supplied as a kit containing a solution and a po wder . The compon ents
must be mixed just before use to ensure optimal performance. Add the
powder to the solution and stir or shake until the powder is completely
dissolved. Once prepared, the solution is stable for 3 months.

• Reagent 3 is the titrant that reacts with the hardness in the sample.

Section 1

• Standards 1 and 2 are used together to perform a multiple-point

calibration. Standard 1 is a 0-mg/L as CaCO
Standard 2 is a 1000-mg/L as CaCO

• The sixth reagent, the Cleaning Solution, cleans the system
during the Prime and Instrument Clean functions. Initially, a different
cleaning solution (Cat. No. 26974-53) may be used to make sure all
parts are wetted.

sodium carbonate solution.

3

sodium carbonate solution.

3

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Section 2 Theory of Operation

The APA 6000™ High Range Har dness Process Analyzer is designed to
provide reproducible results through consistent solution handling. Every step
in an analysis is performed the same way each time, ensuring accurate
results. Accuracy can be v erified and estab lished by measuring grab samples
with a known concentration of analyte.

These steps describe how the analyzer works:

1. The instrument aspirates sample into the holding coil.

2. Appropriate reagents are aspirated.

3. Sample and reagents are premixed in a mixing chamber.

4. The sample-reagent mixture is dispensed into the reaction coil, then

the detector.

5. The mixture flows through the detector and the color is measured.

2.1 Method of Analysis

The sample is treated with a Magnesium-CDTA masking agent at acidic pH,
to eliminate both carbonate/bicarbonate and heavy metal interferences. The
treated sample is then mixed with an indicator/ buffer solution at a higher pH.

Some of the sample/buffer/indicator mixture is aspirated from the mixer and
delivered to the detector via the reaction coil. The remainder of the mixture
then a slug of EDTA titrant is aspirated and delivered to the detector via the
reaction coil.

As the mixture trav el s through t he reaction coil, the titr ant becomes di spersed
through the sample/buffer/indicator mixture on both sides of the titrant slug,
and forms a gradient of EDTA concentration. There will be a small volume of
fluid on both sides of the titran t peak and wh ere the EDTA quantitatively binds
all hardness present, the indicator changes color.

As the fluid flows through the detector, its absorbance is recorded, producing
a characteristic titration peak. The peak width is determined from the
inflection point on both sides of the peak. The instrument calibr ate s us ing tw o
standards to establish a multi-point calibration curve.

In the analysis, segments of untreated sample are kept acidic to assure that
no precipitation occurs in the system.

The measurement cycle follows these basic steps:

1. The analyzer rinses out the holding coil, mixer, and reaction coil in two
steps with acidified sample.

2. Sample is pulled into the holding coil, followed by masking reagent.

6200018theory.fm Theory of Operation

3. This mixture is dispensed into the mixer and stirred. The mixer is filled
in two strokes of the autoburette to assure only representative sample
is in the mixer.

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Section 2

4. A por tio n of th e so lutio n in the mi xer is aspirated out and the

buffer/i ndicator reagent is added. This so lution aliquot and the reagen t are
both dispensed back into the mixer.

5. The solution in the mixer ma y now start to turn red.

6. Some of the solution is aspirated from the mixer and sent to the detector

to prime the reaction coil.

7. The rest of the solution is aspirated from the mixer, followed by a slug of
titrant reagent, and sent to the detector for titrimetric measurement using
a 612 nm LED and a 600 nm filter.

8. As the titrant disperses in the rea cti on coil, a plu g of blue solution may be
seen going through the detector.

The use of inflection points in the titrimetric measurement eliminates the need
for a reference measurement, even for colored samples. Table 2 lists the port
numbers and their function.

Table 2 Port Functions For High Range Hardness Analysis

Port # Function Port # Function

2.2 Reagent Consumption

The rate of reagent use depends on man y factors, including the number of
times the instrument cycles, calibration frequency, and the number of clean
cycles. Table 3 provides the approximate volumes (in mL) of the reagents
consumed with each type of function per cycle.

Solution Measurement Calibration Cleaning

Sample 5.07 0 2.0
Reagent 1 0.140 1.12 0
Reagent 2 0.16 2.56 0
Reagent 3 0.10 1.6 0
Standard 1 0 64.2 0
Standard 2 0 35.4 0
Cleaning Solution 0 0 6.8

1 Detector 6 Waste
2 Sample 1 7 Reagent 3
3 Sample 2 8 Reagent 2 (indicator)
4 Standard 1 9 Reagent 1
5 Standard 2 10 Mixer

Table 3 Reagent Consumption in mL

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Reagent Consumption

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Section 3 Sequence of Instrument Events

Table 4 Initialization

Valve Position Volume (µL) Autoburette Action

Mixer 1000 Aspirate

Waste 1000 Dispense

Mixer 800 Aspirate
Mixer 300 Aspirate

Waste 1100 Dispense

Between ports 1600 Aspirate

Detector 1000 Dispense
Detector 600 Dispense

Table 5 Measurement Mode

Valve Position Volume (µL) Autoburette Action

Sample 500 Aspirate

Mask acid 50 Aspirate

Sample 450 Aspirate

Mixer 1000 Dispense
Mixer 950 Aspirate
Mixer 100 Aspirate

Waste 1050 Dispense

Sample 1500 Aspirate

Mask acid 50 Aspirate

Mixer 1000 Dispense
Mixer 950 Aspirate
Mixer 100 Aspirate

Detector 600 Dispense

Waste 1000 Dispense

Sample 1600 Aspirate

Mixer 850 Dispense

Waste 750 Dispense

Sample 1580 Aspirate

Mixer 0 Depressurize

Mask acid 20 Aspirate

Mixer 850 Dispense

Waste 750 Dispense

Sample 760 Aspirate

Mask acid 20 Aspirate

Sample 260 Aspirate

Mixer 400 Aspirate

Buffer/Indicator 160 Aspirate

Mixer 700 Dispense

Waste 900 Dispense

Mixer 1200 Aspirate

Between ports 100 Aspirate

Detector 600 Dispense

Mixer 600 Aspirate

Titrant 100 Aspirate

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Page 15

Section 3

Valve Position Volume (µL) Autoburette Action

Detector 1400 Dispense

Valve Position Volume (µL) Autoburette Action

Detector 1000 Dispense

Between ports 1600 Aspirate

Detector 1600 Dispense

Between ports 1600 Aspirate

Detector 1600 Dispense

Between ports 1600 Aspirate

Between ports 400 Aspirate

Between ports 1600 Aspirate

Detector 1600 Dispense

Detector 1600 Dispense

Detector 1600 Dispense

Detector 1600 Dispense

Detector 400 Dispense

Table 5 Measurement Mode (continued)

Mixer 250 Aspirate

Waste 250 Dispense

Table 6 Cleaning

Mixer 1000 Aspirate

Mixer 1600 Dispense

Mixer 400 Dispense

Mixer 1600 Aspirate

Mixer 1600 Aspirate

Sample 1600 Aspirate

Mixer 1600 Dispense

Sample 400 Aspirate

Mixer 400 Dispense
Mixer 1600 Aspirate

Mixer 400 Aspirate

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Sequence of Instrument Events

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Section 3

Table 7 Prime All

Valve Position Volume (µL) Autoburette Action

Between ports 1600 Aspirate

Waste 1600 Dispense

Between ports 1600 Aspirate

Waste 1600 Dispense

Mask acid 1000 Aspirate

Waste 1000 Dispense

Buffer/Indicator 1000 Aspirate

Waste 1000 Dispense
Titrant 1000 Aspirate
Waste 1000 Dispense

Between ports 1600 Aspirate

Waste 1600 Dispense

Standard 2 1000 Aspirate

Waste 1000 Dispense

Standard 1 1000 Aspirate

Waste 1000 Dispense

Between ports 1600 Aspirate

Waste 1600 Dispense

6200018script.fm Sequence of Instrument Events

Page 17

Section 3

Valve Position Volume (µL) Autoburette Action

CAL STEP 1

Standard 1 500 Aspirate

Mask acid 50 Aspirate

Standard 1 450 Aspirate

Standard 1 1500 Aspirate

Mask acid 50 Aspirate

Detector 600 Dispense

Standard 1 1600 Aspirate

Standard 1 1495 Aspirate
Standard 2 85 Aspirate

Mask acid 20 Aspirate

Standard 1 760 Aspirate

Mask acid 20 Aspirate

Standard 1 260 Aspirate

Buffer/Indicator 160 Aspirate

Between ports 100 Aspirate

Detector 600 Dispense

Detector 1400 Dispense

Table 8 Calibration

Mixer 1000 Dispense
Mixer 950 Aspirate
Mixer 100 Aspirate

Waste 1050 Dispense

Mixer 1000 Dispense
Mixer 950 Aspirate
Mixer 100 Aspirate

Waste 1000 Dispense

Mixer 850 Dispense

Waste 750 Dispense

Mixer 0 Depressurize

Mixer 850 Dispense

Waste 750 Dispense

Mixer 400 Aspirate

Mixer 700 Dispense

Waste 900 Dispense

Mixer 1200 Aspirate

Mixer 600 Aspirate

Titrant 100 Aspirate

Mixer 250 Aspirate

Waste 250 Dispense

Page 18

Sequence of Instrument Events

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CAL STEP 2

Section 3

Table 8 Calibration (continued)

Valve Position Volume (µL) Autoburette Action

Standard 1 500 Aspirate

Mask acid 50 Aspirate

Standard 1 450 Aspirate

Mixer 1000 Dispense
Mixer 950 Aspirate
Mixer 100 Aspirate

Waste 1050 Dispense

Standard 1 1500 Aspirate

Mask acid 50 Aspirate

Mixer 1000 Dispense
Mixer 950 Aspirate
Mixer 100 Aspirate

Detector 600 Dispense

Waste 1000 Dispense

Standard 1 1600 Aspirate

Mixer 850 Dispense

Waste 750 Dispense
Standard 1 1410 Aspirate
Standard 2 170 Aspirate

Mixer 0 Depressurize

Mask acid 20 Aspirate

Mixer 850 Dispense

Waste 750 Dispense
Standard 1 760 Aspirate

Mask acid 20 Aspirate

Standard 1 260 Aspirate

Mixer 400 Aspirate

Buffer/Indicator 160 Aspirate

Mixer 700 Dispense

Waste 900 Dispense

Mixer 1200 Aspirate

Between ports 100 Aspirate

Detector 600 Dispense

Mixer 600 Aspirate

Titrant 100 Aspirate

Detector 1400 Dispense

Mixer 250 Aspirate

Waste 250 Dispense

6200018script.fm Sequence of Instrument Events

Page 19

Section 3

Valve Position Volume (µL) Autoburette Action

CAL STEP 3

Standard 2 500 Aspirate

Mask acid 50 Aspirate

Standard 2 450 Aspirate

Standard 2 1500 Aspirate

Mask acid 50 Aspirate

Detector 600 Dispense

Standard 2 1600 Aspirate

Standard 1 1580 Aspirate

Mask acid 20 Aspirate

Standard 1 760 Aspirate

Mask acid 20 Aspirate

Standard 1 260 Aspirate

Buffer/Indicator 160 Aspirate

Between ports 100 Aspirate

Detector 600 Dispense

Detector 1400 Dispense

Table 8 Calibration (continued)

Mixer 1000 Dispense
Mixer 950 Aspirate
Mixer 100 Aspirate

Waste 1050 Dispense

Mixer 1000 Dispense
Mixer 950 Aspirate
Mixer 100 Aspirate

Waste 1000 Dispense

Mixer 850 Dispense

Waste 750 Dispense

Mixer 0 Depressurize

Mixer 850 Dispense

Waste 750 Dispense

Mixer 400 Aspirate

Mixer 700 Dispense

Waste 900 Dispense

Mixer 1200 Aspirate

Mixer 600 Aspirate

Titrant 100 Aspirate

Mixer 250 Aspirate

Waste 250 Dispense

Page 20

Sequence of Instrument Events

6200018script.fm

CAL STEP 4

Section 3

Table 8 Calibration (continued)

Valve Position Volume (µL) Autoburette Action

Standard 2 500 Aspirate

Mask acid 50 Aspirate

Standard 2 450 Aspirate

Mixer 1000 Dispense
Mixer 950 Aspirate
Mixer 100 Aspirate

Waste 1050 Dispense
Standard 2 1500 Aspirate

Mask acid 50 Aspirate

Mixer 1000 Dispense
Mixer 950 Aspirate
Mixer 100 Aspirate

Detector 600 Dispense

Waste 1000 Dispense
Standard 2 1600 Aspirate

Mixer 850 Dispense

Waste 750 Dispense
Standard 2 1580 Aspirate

Mixer 0 Depressurize

Mask acid 20 Aspirate

Mixer 850 Dispense

Waste 750 Dispense
Standard 2 760 Aspirate

Mask acid 20 Aspirate

Standard 2 260 Aspirate

Mixer 400 Aspirate

Buffer/Indicator 160 Aspirate

Mixer 700 Dispense

Waste 900 Dispense

Mixer 1200 Aspirate

Between ports 100 Aspirate

Detector 600 Dispense

Mixer 600 Aspirate

Titrant 100 Aspirate

Detector 1400 Dispense

Mixer 250 Aspirate

Waste 250 Dispense

6200018script.fm Sequence of Instrument Events

Page 21

Section 4 Parameter Specific Functions

4.1 Calibration History

This option allows you to review past calibration data.

1. Press the MENU key to start from the Main Menu.

2. Select Sensor Menu and press ENTER.

3. Select the sensor by name and press ENTER.

4. Select Calibration and press ENTER.

5. Select Cal History and press ENTER.

6. A pop-up box will appear with the calibration date and time of the seven

most recent calibrations . Select Review Next Cal to step through the
“pages” of the calibration history. After the last calibration, press ENTER
to return to the previous menu. To exit the Cal History Menu, press EXIT.

The calibration is cubic and is based on 50, 100, 500, and 10 00 mg/L as
CaCO
1000 mg/L as CaCO
calibrations will include the concentration of the 50 and 500 ppm calibration
points. Thevalues are based on the previous calibration curve and applied to
the standards on the current calibration.

standards that are prepared by the analyzer from the 0 and

3

standards. Data displayed for the se ven most recent

3

4.2 Measurement Options

The analyzer allows several options for the display of concentration values.
The units can be changed. Available options are mg/L, ppm, gr/gal, and Gdh.

Note: If a Digital Display Module (DDM) is used, select SENSOR to DISPLAY in the

Important Note: Changing the displayed units will cause the stored data for the

Network Menu to set the output of the DDM.

AquaTrend channel on which the units were changed to be erased.

Page 22

Parameter Specific Functions

6200018menu.fm

Section 5 Bench Method Procedure

FILL LINEFILL LINE

5.1 Standardization

Standardize Reagent 3 with Standard 2 (1000 mg/L as CaCO3) to determine
the titer value of Reagent 3 be f ore testin g samples f or tot al hardness . Perf orm
a standardization before any sample analysis, as reagents may change
over time.

5.2 Standardization Procedure

1. Fill a 25-mL buret with

Reagent 3. This will be
used to titrate in step 6.

5. Using a graduated
cylinder, add 8 mL of
Reagent 2. Swirl to mix.

Note: Prepare Reagent 2 by
mixing one bottle of Indicator
Powder into 1 L of Buffer
Solution. Reagent 2 can then
be kept for approximately
3months.

2. Use a volumetric pipet
to transfer 20.00 mL
of Standard 2 solution
into a clean 250-mL
Erlenmeyer flask.

6. Swirl the flask while
titrating with Reagent 3
from red to pure blue.

3. Dilute to about the
100-mL mark with
deionized water.

7. Record the volume of
Reagent 3 required.

Reagent 3 Titer (M)

4. Using a marked
dropper, add 1 mL of
Reagent 1.
Swirl to mix.

8. Calculate the titer of
Reagent 3 using the
equation below:

---------------------------------------------------------------=

Reagent 3 Volume (mL)

0.2

6200018bench.fm Bench Method Procedure

Page 23

Section 5

Repeat

steps 1-8 twice.

Average the three
values for the titer

of Reagent 3

9. Repeat steps 1-8 twice. 10. Use the average
value for the titer of
Reagent 3.

5.3 Testing Samples for Total Hardness

Refer to Table 9 to choose between using a buret or a digital titrator,
depending on the sample concentration.

Use the information in Tabl e 10 to determine the correct sample volume and
pipet size fo r the digital titrator procedure.

Use the information in Tabl e 11 to determine the correct sample volume and
pipet size for the buret titration procedure.

Table 9 Choosing a Titration Method

Sample Concentration

(mg/L as CaCO3)

10 – 100 Digital Titrator

100 – 1000 Buret

Titration Method

Table 10 Required Sample Volume for Digital Titrator Procedure

Sample Concentration

(mg/L as CaCO3)

10 – 50 20

50 – 100 10

Sample V o lume (mL)

Table 11 Required Sample Volume for Buret Titration Procedure

Sample Concentration

(mg/L as CaCO

100 – 250 100
250 – 500 50

500 – 1000 20

)

3

Sample V o lume (mL)

Page 24

Testing Samples for Total Hardness

6200018bench.fm

5.3.1 Total Hardness Digital Titrator® Method

FILL LINE

Section 5

Refer to Tabl e

10 on page 24.

1. If a Digital Titrator

is used, fill a clean and
empty titration cartridge
with Reagent 3.

5. Using the volumetric

pipet, transfer the sample
volume from Table 10 into
a clean 250-mL
Erlenmeyer flask.

2. Insert a clean delivery
tube into the titration
cartridge. Attach the
cartridge to the titrator
body.

6. Dilute to about the
100-mL mark with
deionized water.

3. Turn the delivery knob
to eject a few drops of
Reagent 3. Reset the
counter to zero and wipe
the tip.

7. Using a marked
dropper, add 1 mL of
Reagent 1. Swirl to mix.

4. Refer to Table 10 to
choose the size of the
volumetric pipet,
depending on sample
concentration.

8. Using a graduated
cylinder, ad d 8 mL of
Reagent 2. Swirl to mix.

Note: Prepare Reagent 2 by
mixing one bottle of Indicator
Powder into 1 L of Buffer
Solution. Reagent 2 can then
be kept for approximately
3 months.

9. Swirl the flask while

titrating with Reagent 3

10. Record the number of
digits required.

from red to pure blue.

Sample Concentration mg/L as CaCO

6200018bench.fm Testing Samples for Total Hardness

11. Calculate the sample
concentration using the
equation below:

()

125 Digits Required Reagent 3 Titer M()××

--------------------------------------------------------------------------------------------------------------------- -=

3

Sample Volume (mL)

Page 25

Section 5

FILL LINEFILL LINE

5.3.2 Total Hardness Buret Method

Refer to Tabl e

11 on page 24.

1. If a buret is used, fill

a 25-mL buret with
Reagent 3.

5. Using a marked

dropper, add 1 mL of
Reagent 1.
Swirl to mix.

2. Refer to Table 11 to
choose the size of the
volumetric pipet,
depending on sample
concentration.

6. Using a graduated
cylinder, add 8 mL of
Reagent 2. Swirl to mix.

Note: Prepare Reagent 2 by
mixing one bottle of Indicator
Po w d er in to 1 L of Buffer
Solution. Reagent 2 can be
kept for approximately 3
months.

3. Using the volumetric
pipet, transfer the sample
volume from T able 11 into a
clean 250-mL Erlenmeyer
flask.

7. Swirl the flask while
titrating with Reagent 3
from red to pure blue.

4. Dilute to about the
100-mL mark with
deionized water,
if necessary.

8. Record the volume
required.

9. Calculate the sample

concentration using the
equation below:

Sample Concentration mg/L as CaCO

Page 26

Testing Samples for Total Hardness

()

100000 Volume Required mL()× Reagent 3 titer M()×

-------------------------------------------------------------------------------------------------------------------------------------------------=

3

Sample Volume mL()

6200018bench.fm

Section 6 Replacement Parts

Required Reagents for APA 6000™ High Range Hardness Analyzer

APA 6000™ High Range Hardness Reagent 1.......................................... .... ... ... ........................ 1 L..........27935-53

APA 6000™ High Range Hardness Reagent 2 Kit........................ .... ... ... ................................... e ach..........27936-00

APA 6000™ High Range Hardness Reagent 3.......................................... .... ... ... ........................ 1 L..........27937-53

APA 6000™ High Range Hardness Standard 1, 0 mg/mL........................................................... 1 L..........27932-53

APA 6000™ High Range Hardness Standard 2, 1000 mg/L........................................................ 1 L..........27933-53

Wash Solution.............................................................................................................................. 1 L..........28764-53

Required Reagents for Bench Method

Quantity Required

Description Per Test Unit Cat. No.

APA 6000™ High Range Hardness Reagent 1.......................................... ... 1 mL...................... 1 L..........27935-53

APA 6000™ High Range Hardness Reagent 2 Kit........................ .... ... ... ......8 mL....................e ach..........27936-00

APA 6000™ High Range Hardness Reagent 3.......................................... 5–20 mL................... 1 L..........27937-53

APA 6000™ High Range Hardness Standard 2, 1000 mg/L................60 mL (cal. only)............. 1 L..........27933-53

Water, deionized .................................................. ... ... ................................<100 mL................... 4 L..............272-56

Required Apparatus for Bench Method

Buret, 25 mL, Class A, certified ....................................................................... * .......................each..........26365-40

Cylinder, graduated, 10 mL..............................................................................1.......................each.............. 508-38

Delivery tubes for the Digital Titrator, 90° with J-hook ..................................... *......................5/pkg..........41578-00

Digital Titrator................................................................................................... * .......................each..........16900-01

Digital Titrator cartridge, empty........................................................................ *.......................each.......... 14495-01

Dropper, glass with 0.5 and 1-mL mark ...........................................................1......................5/pkg.......... 14197-05

Flask, Erlenmeyer, 250 mL ..............................................................................1.......................each.......... 24894-46

Pipet, volumetric, 10 mL, Class A ................................................................... * .......................each..........14515-38

Pipet, volumetric, 20 mL, Class A ............................................................1 (cal. only)...............each.......... 14515-20

Pipet, volumetric, 50 mL, Class A ................................................................... * .......................each..........14515-41

Pipet, volumetric, 100 mL, Class A ................................................................. * .......................each..........14515-42

Pipet bulb, 3-valve............................................................................................1.......................each.......... 12189-00

Wash bottle, 500 mL........................................................................................1.......................each.............. 620-11

Optional Apparatus

Bottles, storage, polyethylene, 60 mL.....................................................................................12/pkg..........20870-71

Kimwipes, 11 x 22 cm (4.5 x 8.5 inches).............. ... ... ... ... .....................................................280/box..........20970-00

Replacement Parts

Mixer Module Assembly, APA 6000, 1-mL .................................................................................each..........51021-00

Colorimeter Module, 600 nm......................................................................................................each.......... 62060-04

* The titration method and necessary apparatus are sample concentration dependent. Refer to Section 5.3 on page 24.

6200018parts.fm Replacement Parts

For common APA 6000 Parts and Accessories, please see the APA 6000
Process Analyzer Installation and Maintenance Manual, Cat. No. 62005-18.

Page 27

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