Hach Pocket Colorimeter II, 59530-01, 59530-51, 59530-12 Instruction Manuals

Page 1
59571-88
POCKET COLORIMETER™ II
ANALYSIS SYSTEMS
INSTRUCTION MANUAL
Bromine (Br)
Chlorine Dioxide (ClO
2
)
2
) / pH
© Hach Company, 2004–2006. All rights reserved. Printed in the U.S.A. te/dk 9/06 4ed
Page 2
1—2
Important Note
This manual is intended for use with the following Pocket Colorimet er™ II instruments:
The Pocket Colorimeter™ II instruments listed above are not interchangeable.
Bromine Cat. No. 59530-01 Chlorine Dioxide Cat. No. 59530-51 Chlorine / pH Cat. No. 59530-12
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1—3
Table of Contents
Safety Precautions............................................................................................... 1—7
Laboratory Safety............................................................................................... 1—7
Use of Hazard Information................................................................................ 1—7
Precautionary Labels........ ....... ....... ....................................................................1— 8
Specifications......................................................................................................... 1—9
Instrument Keys and Display...........................................................................1—11
Instrument Cap Cord.........................................................................................1—12
Bromine, Total, LR..............................................................................................1—15
Measuring Hints ...............................................................................................1—15
Sampling and Storage......................................................................................1—22
Accuracy Check................ ....... .............................................................. ...........1—22
Interferences......................................................................................................1—24
Method Performance........................................................................................1—26
Bromine, Total, HR.............................................................................................1—27
Measuring Hints ...............................................................................................1—27
Sampling and Storage......................................................................................1—31
Accuracy Check................ ....... .............................................................. ...........1—31
Interferences......................................................................................................1—33
Page 4
1—4
Table of Contents, continued
Method Performance........................................................................................1—35
Summary of Method.........................................................................................1—35
Replacement Parts (LR and HR)......................................................................1—35
Chlorine, Free and Total, HR..........................................................................1—39
Measuring Hints................................................................................................1—39
Accuracy Check............................................. ....................................................1—44
Interferences......................................................................................................1—46
Spec
Secondary Standards............................................................................1—49
Method Performance........................................................................................1—49
Summary of Method.........................................................................................1—49
Replacement Parts.............................................................................................1—50
Chlorine Dioxide..................................................................................................1—53
Measuring Hints................................................................................................1—53
Sampling and Storage......................................................................................1—61
Accuracy Check............................................. ....................................................1—61
Method Performance........................................................................................1—64
Interferences......................................................................................................1—64
Summary of Method.........................................................................................1—66
Reagents and Apparatus................................................................ ....... ...........1—6 6
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1—5
Table of Contents, continued
pH..............................................................................................................................1—69
Measuring Hints ...............................................................................................1—69
Accuracy Check................ ....... .............................................................. ...........1—74
Method Performance........................................................................................1—74
Standard Calibration Adjust ...........................................................................1—75
Summary of Method........................................................................................1—75
Replacement Parts............................................................................................1—76
Instrument Operation.........................................................................................2—3
Key Functions..................................................................................................... 2—3
Menu Selections.............................. ....................................................................2— 4
Switching Ranges............................................................................................... 2—4
Setting the Time ................................................................................................. 2—4
Recalling Stored Measurements........................................................................ 2—5
Battery Installation............................................................................................. 2—6
Error Codes.............................................................................................................. 2—9
Error Messages.................................................................................................... 2—9
Standard Calibration Adjust..........................................................................2—13
Page 6
1—6
Table of Contents, continued
User-Entered Calibration.................................................................................2—15
Overview............................................................................................................2—15
Calibration Procedure Using Prepared Standards.........................................2—17
Entering a Predetermined Calibration Curve.......... .......................................2—20
Editing a User-entered or Factory Calibration Curve...................................2—22
Exiting the Calibration Routine......................... .............................................2—24
Deleting Calibration Points.......................... ....... ...... .......................................2—24
Retrieving the Factory Calibration ............................................... ..................2 —25
Maximum/Minimum Displayed Value....................................................... ....2—26
Certification..........................................................................................................2—28
How to Order........................................................................................................2—35
Repair Service.......................................................................................................2—37
Warranty.................................................................................................................2—38
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1—7
Safety Precautions
Please read this entire manual before unpacking, setting up, or operating this instrument. Pay particular attention to all danger and caution statements. Failure to do so could result in serious injury to the operator or damage to the equipment.
To ensure the protection provided by this equipment is not impaired, do not use or install this equipment in any manner other than that which is specified in this manual.
Laboratory Safety
As part of good laboratory practice, pl eas e familiarize yourself with the reagents used in these procedures. Read all product labels and the m aterial safety data sheets (MSDS) before using them. It is always good practice to wear safety glasses when handling chemicals. Foll ow instructions carefully. Rinse thoroughly if contact occurs. If you have questions about reagents or procedures, please contact the manufacturer or distributor.
Use of Hazard Information
If multiple hazards exist, this manu al wi ll use th e sign al wo rd (Danger, Caution, Note) corresponding to the greatest hazard.
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1—8
Safety Precautions, continued
DANGER Indicates a potentially or imminently hazardous situation which, if not avoided, could result in death or serious injury.
CAUTION Indicates a potentially hazardous situation that may result in minor or moderate injury.
NOTE Information that requires special emphasis.
Precautionary Labels
Please pay particular attention to labels and tags attached to the instrument. Personal injury or damage to the instrument could occur if not observed.
This symbol, if noted on the instrume n t, referen ces the instruct io n manual
for operational and/or safety inform ation.
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1—9
Specifications
Lamp: Light emitting diode (LED) Detector: Silicon photodiode Photometric precision: ± 0.0015 Abs Filter bandwidth: 15 nm Wavelength: 528 nm Absorbance range: 0–2.5 Abs Dimensions: 3.2 x 6.1 x 15.2 cm (1.25 x 2.4 x 6 inches) Weight: 0.2 kg (0.43 lb) Sample cells: 25 mm (10 mL), 1 cm (10 mL), AccuVac
®
Ampuls
Operating conditions: 0 to 50 °C (32 to 122 °F); 0 to 90% relative humidity (noncondensing)
Power supply: Four AAA alkaline batteries; approximate life is 2000 tests*
* Backlight usage will decrease battery life.
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1—10
OPERATION
DANGER
Handling chemical samples, standards, and reagents can be dangerous. Review the necessary Material Safety Data Sheets and become familiar with all safety procedures before handling any chemicals.
DANGER
La manipulation des échantillons chimiques, étalons et réactifs peut être danger euse. Lir e les Fiches de Données de Sécurité des Produits (FDSP) et se familiariser avec toutes les procédures de sécurité avant de manipuler tous les produits chimiques.
PELIGRO
La manipulación de muestras químicas, estándares y reactivos puede ser peligro s a. Revi se las fichas de seguridad de materiales y familiarícese con los procedimientos de seguridad antes de manipular productos químicos.
GEFAHR
Das Arbeiten mit chemischen Proben, Standards und Reagenzien ist mit Gefahren verbunden. Es wird dem Benutzer dieser Produkte empfohlen, sich vor der Arbeit mit sicheren Verfahrensweisen und dem richtigen Gebrauch der Chemikalien vertraut zu machen und alle entsprechenden Materialsicherheitsdatenblätter aufmerksam zu lesen.
PERIGO
A manipulação de amostras, padrões e reagentes químicos pode ser perigosa. Reveja a folha dos dados de segurança do material e familiarize-se com todos os procedimentos de segurança antes de manipular quaisquer produtos químicos.
PERICOLO
La manipolazione di campioni, standard e reattivi chimici può essere 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 manip olare ogni prodotto chimico.
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1—11
Instrument Keys and Display
Item Description
1 POWER/BACKLIGHT Key 2
ZERO/SCROLL Key
3
MENU Key
4 Numeric Display 5 Range Indicator 6 Range Indicator 7 Menu Indicator 8 Calibration Adjusted Indicator 9 Battery Low Indicator
10
READ/ENTER Key
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1—12
Instrument Cap Cord
The instrument cap for the Pocket Colorimeter™ II doubles as a light shield. Accurate measurements cannot be obtained unless the sample or blan k is covered with the cap. Use the instrument cap cord to secure the cap to the body of the colorimeter and prevent loss of the cap. See Figu re 1 on page 1—13.
1. Loop the instrument cap cord through the ring on the cap.
2. Remove the battery compartment cover. Press the knotted end of the cord into
the hole indicated by the arro w.
3. Slide the cord into the slot on the battery compartment cover. Snap the cover into place.
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1—13
Instrument Cap Cord, continued
Figure 1 Attaching the Instrument Cap Cord
Page 14
1—14
Page 15
1—15
Bromine, Total, LR (0.05 to 4.50 mg/L Br
2
)
Method 8016
For water, wastewater, and seawater
DPD Method* (PermaChem® Powder Pillows or AccuVac® Ampuls)
Measuring Hints
Analyze samples immediately . Do not use plastic containers to collect sample s.
Note:
The Pocket Colorimeter™ II is designed to measure solutions contained in sample cells.
DO NOT
dip the meter in the sample or pour the sample directly into the cell holder.
Note:
If the sample temporarily turns yellow after reagent addition, or if the display shows overrange (page 2—10), dilute a fresh sample and repeat the test. A slight loss of bromine may occur because of the dilution. Multiply the result by the appropriate dilution factor.
* Adapted from Standard Methods for Examination of Water and Wastewater.
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1—16
Bromine, Total, LR, continued
Bromine, Total, Low Range (using Powder Pillows)
1.Fill a 10-mL sample cell
sample (the blank). Cap.
Note:
Samples must be analyzed immediately and cannot be preserved for later analysis.
2.Pr ess the POWER key to
turn the meter on. The arrow sh ould indicate
the low range channel (LR).
Note:
See page 2—4 for information on selecting the correct range channel.
3.Remove the instrument
cap. Place the blank in the cell holder. Cover the blank with the instrument cap.
Note:
Wipe excess liquid and fingerprints from the sample cells.
Page 17
1—17
Bromine, Total, LR, continued
4.Press ZERO/SCROLL.
The display will show “- - - -” then “0.00”.
Remove the blank fro m the cell holder.
5.Fill a second sample cell
to the 10 mL line with sample. Wipe off any liquid or fingerprints.
6.Ad d the cont ents of one
DPD Total Chlorine Powder Pillow to the sample cell (the prepared sample).
Note:
The SwifTest™ Dispenser for total chlorine can be used in place of the powder pillow.
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1—18
Bromine, Total, LR, continued
7.Cap and s hake gently for
20 seconds.
Note:
Shaking dissipates bubbles that may form in samples with dissolved gases.
Note:
A pink color will develop if bromine is present.
Note:
Wipe liquid off sample
cells.
8.Place the prepared
sample in the cell holder and cover with the instrument cap. Wait at least three but no more than six minutes after adding the DPD Total Chlorine Pillow.
Note:
Accuracy is not affected by undissolved powder.
9.Press READ/ENTER.
The display will show “- - - -”, followed by results in mg/L bromine.
Page 19
1—19
Bromine, Total, LR, continued
Bromine, Total, Low Range (using AccuVac® Ampuls)
1.Fill a 10-mL sample
cell with sample (the blank). Cap. Collect at least 40 mL of sample in a 50-mL beaker.
Note:
Samples must be analyzed immediately and cannot be preserved for later analysis.
2.Press the POWER key
to turn the meter on. The arrow should indicate
the low range channel (LR).
Note:
See page 2—4 for information on selecting the correct range channel.
3.Remove the instrument
cap. Place the blank in the cell holder. Cover the blank with the instrument cap.
Note:
Wipe excess liquid and fingerprints from the sample cells.
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1—20
Bromine, Total, LR, continued
4.Press ZERO/SCROLL.
The display will show “- - - -” then “0.00”.
Remove the blank from the cell holder.
5.Fill a DPD Total
Chlorine Reagent AccuV ac Ampul with sample. Keep the tip of the ampule immersed until the ampule fills completely.
6.Quickly invert the
ampul several times to mix. Wipe off any liquid or fingerprints.
Note:
A pink color will
form if bromine is present.
Note:
Accuracy is not affected by undissolved powder.
Page 21
1—21
Bromine, Total, LR, continued
7.Place the prepared
sample in the cell holder and cover with the instrument cap. Wait at least three but no more than six minutes after filling the ampule.
Note:
Wipe liquid off
sample cells.
8.Press READ/ENTER.
The display will show “- - - -”, followed by results in mg/L bromine.
Page 22
1—22
Bromine, Total, LR, continued Sampling and Storage
Analyze samples immediately. Do not collect samples in plasti c con tai ners.
Accuracy Check
Standard Additions Method
1. Snap the neck off a low range Chlorine Standard Solution PourRite® Ampule, 20–30 mg/L Cl
2
.
2. Use a TenSette
®
pipet to add 0.1, 0.2, and 0.3 mL of standard to three 10-mL samples. Swirl gently to mix. (For AccuVac Ampuls, use 0.3, 0.6, and 0.9 mL of standard and a 30-mL sample in a 50-mL beaker.)
3. Analyze each sample as described in the procedure. Each 0.1 mL of stan da rd will cause an incremental increase in the apparent bromine concentration. The exact value depends on the concentration of the ampule standard. Check the certificate enclosed with the standard ampules for the chlorine concentration. Multiply the expected chlorine concentration by 2.25 to determine the expected increase in bromine concentration.
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Bromine, Total, LR, continued
Standard Solution Method
Standard solutions for bromine or chlorine are difficult and time-consuming to prepare. Errors can occur if attention to detail is not addressed during preparation of the standards. Hach Company prepares the calibration curve under rigorous analytical laboratory conditions. Hach strongly recommends using the facto ry calibration.
A user calibration or a user-prepared br omine standard may be required by a regulatory official or agency. Two options are available on the Pocket Colorimeter™ II to meet this requirement.
A bromine standard may be prepared and used to validate th e calib ration curve using the Standard Calibration Adjust feature (see page 2—13 for more information.). The concentration of the prepared standard must be determined with an alternate instrument such as a spectrophotometer, colorimeter, amperometric titration, or by using another alternate method. The concentration of the bromine standard for the low range procedure must be between 2.00 and 4.00 mg/L bromine.
In addition, a user-generated calibration curve can be made and programmed into the Pocket Colorimeter™ II. See User-Entered Calibration on page 2—15.
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Bromine, Total, LR, continued
If a chlorine standard is used, multiply its concentration by 2.25 to determine the equivalent bromine concentration.
Interferences
Interfering Substance
Interference Levels and Treatments
Acidity Greater than 150 mg/L CaCO3. May not develop full color or
color may fade instantly. Neutralize to pH 6–7 with 1 N Sodium Hydroxide. Determine amount to be added on separate 10-mL sample, then add the same amount to the sample being tested. Correct for the additional volume.
Alkalinity Greater than 250 mg/L CaCO
3
. May not develop full color or color may fade instantly. Neutralize to pH 6–7 with 1 N Sulfuric Acid. Determine amount to be added on separate 10-mL sample, then add the same amount to the sample being tested. Correct for the additional volume.
Chlorine, Cl
2
Interferes at all levels
Page 25
1—25
Bromine, Total, LR, continued
Hardness No effect at less than 1,000 mg/L as CaCO
3
Iodine, I
2
Interferes at all levels
Manganese, Oxidized (Mn
4+
, Mn7+) or Chromium, Oxidized (Cr
6+
)
1. Adjust sample pH to 6–7.
2. Add 3 drops Potassium Iodide (30-g/L) (Cat. No. 343-32)
to a 25-mL sample.
3. Mix and wait one minute.
4. Add 3 drops Sodium Arsenite (5-g/L) (Cat. No. 1047-32)
and mix.
5. Analyze 10 mL of the treated sample as described in
the procedure.
6. Subtract the result of this test from the original analysis
result to obtain the correct chlorine concentration. Monochloramine Interferes at all levels. Ozone Interferes at all levels.
Interfering Substance
Interference Levels and Treatments
Page 26
1—26
Bromine, Total, LR, continued Method Performance
Estimated Detection Limit (EDL) = 0.05 mg/L Br
2
Typical Precision (95% confidence interval) = 2.25 ± 0.11 mg/L Br
2
Page 27
1—27
Bromine, Total, HR (0.2 to 10.0 mg/L Br
2
)
Method 8016
For water, wastewater, and seawater
DPD Method* (PermaChem® Powder Pillows)
Measuring Hints
If the bromine concentration is typically less than 4 mg/L, use the low range procedure.
Analyze samples immediately . Do not use plastic containers to collect sample s.
Note:
The Pocket Colorimeter II is designed to measure solutions contained in sample cells.
DO NOT
dip the meter in the sample or pour the sample directly into the cell holder.
* Adapted from Standard Methods for Examination of Water and Wastewater.
Page 28
1—28
Bromine, Total, HR, continued
1.Fill a 1-cm/10-mL
sample cell with sample. Cap. This is the blank.
Note:
Samples must be analyzed immediately and cannot be preserved for later analysis.
2.Pr ess the POWER key to
turn the meter on. The arrow sh ould indicate
the high range channel (HR).
Note:
See page 2—4 for information on selecting the correct range channel.
3.Remove the meter cap.
Place the blank into the cell holder, with the diamond mark facing the back of the cell holder. Cover the cell with the cap.
Note:
Wipe excess liquid and fingerprints from the sample cells.
Page 29
1—29
Bromine, Total, HR, continued
4.Press ZERO/SCROLL.
The display will show “- - - -” then “0.0”.
Remove the blank fro m the cell holder.
5.Fill another 1-cm/1 0-mL
sample cell to the 5-mL line with sample.
6.Add the contents of two
DPD Total Chlorine Powder Pillows to the sample cell (the prepare d sample).
Note:
The SwifTest™ Dispenser for Total Chlorine can be used in place of the powder pillows. Use two dispensations from the dispenser.
Page 30
1—30
Bromine, Total, HR, continued
7.Cap and s hake gently for
20 seconds.
Note:
Shaking dissipates bubbles that may form in samples with dissolved gases.
Note:
A pink color will develop if bromine is present.
Note:
Wipe liquid off sample
cells.
8.Place the prepared
sample in the cell holder and cover with the instrument cap. Wait at least three but no more than six minutes after adding the DPD Total Chlorine Pillows.
Note:
Accuracy is not affected by undissolved powder.
9.Press READ/ENTER.
The display will show “- - - -”, followed by results in mg/L bromine.
10
m
L
5
m
L
Page 31
1—31
Bromine, Total, HR, continued
Note:
If the sample temporarily turns yellow after reagent addition, or if the display shows overrange (page 2—12), dilute a fresh sample and repeat the test. A slight loss of bromine may occur because of the dilution. Multiply the result by the appropriate dilution factor.
Sampling and Storage
Analyze samples immediately. Do not collect samples in plasti c con tai ners.
Accuracy Check
Standard Additions Method
1. Snap the neck off a high range Chlorine Standard Solution V oluette® Ampule, 25–30 mg/L Cl
2
.
2. Use a TenSette
®
pipet to add 0.1, 0.2, and 0.3 mL of standard to three separate
5-mL samples. Swirl gently to mix.
3. Analyze 5 mL of each sample as described in the procedure. Each 0.1 mL of standard will cause an incremental in crease in bromine concentration. The exact value depends on the concentration of the ampule standard. Check the certificate enclosed with the standard ampules for the chlorine concentration. Multiply the expected chlorine concentration by 2.25 to determine the expected increase in bromine concentration.
Page 32
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Bromine, Total, HR, continued
Standard Solution Method
Standard solutions for bromine or chlorine are difficult and time-consuming to prepare. Errors can occur if attention to detail is not addressed during preparation of the standards. Hach Company prepares the calibration curve under rigorous analytical laboratory conditions. Hach stron gly recomm en ds usin g th e factory calibration.
A user calibration or a user-prepared br omine standard may be required by a regulatory official or agency. Two options are available on the Pocket Colorimeter II to meet this requirement.
A bromine standard may be prepared and used to validate the calibration curve using the Standard Calibration Adjust feature (see page 2—13 for more information.). The concentration of the prepared standard must be determined with an alternate instrument such as a spectro ph ot om et er, colorimeter, amperometric titration, or by using another alternate method. The concentration of the bromine standard for the low range procedure must be between 2.00 and 4.00 mg/L bromine and between 2.0 and 8.0 mg/L bromine for the high range procedure.
In addition, a user-generated calibration curve can be made and programmed into the Pocket Colorimeter™ II. See User-Entered Calib rati on on pa ge 2—1 5.
Page 33
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Bromine, Total, HR, continued
If a chlorine standard is used, multiply its concentration by 2.25 to determine the equivalent bromine concentration.
Interferences
Interfering Substance
Interference Levels and Treatments
Acidity Greater than 150 mg/L CaCO3. May not develop full color or
color may fade instantly. Neutralize to pH 6–7 with 1 N Sodium Hydroxide. Determine amount to be added on separate 10-mL sample, then add the same amount to the sample being tested. Correct for the additional volume.
Alkalinity Greater than 250 mg/L CaCO
3
. May not develop full color or color may fade instantly. Neutralize to pH 6–7 with 1 N Sulfuric Acid. Determine amount to be added on separate 10-mL sample, then add the same amount to the sample being tested. Correct for the additional volume.
Chlorine, Cl
2
Interferes at all levels
Page 34
1—34
Bromine, Total, HR, continued
Hardness No effect at less than 1,000 mg/L as CaCO
3
Iodine, I
2
Interferes at all levels
Manganese, Oxidized (Mn
4+
, Mn7+) or Chromium, Oxidized (Cr
6+
)
1. Adjust sample pH to 6–7.
2. Add 3 drops Potassium Iodide (30-g/L) (Cat. No. 343-32) to
a 25-mL sample.
3. Mix and wait one minute.
4. Add 3 drops Sodium Arsenite (5-g/L) (Cat. No. 1047-32)
and mix.
5. Analyze 10 mL of the treated sample as described in
the procedure.
6. Subtract the result of this test from the original analysis
result to obtain the correct chlorine concentration. Monochloramine Interferes at all levels. Ozone Interferes at all levels.
Interfering Substance
Interference Levels and Treatments
Page 35
1—35
Bromine, Total, HR, continued
Method Performance
Estimated Detection Limit (E DL) = 0.2 m g/L Br
2
Typical Precision (95% confidence interva l) = 11.3 ± 0.5 mg/L Br
2
Summary of Method
Bromine residuals react with DPD (N,N-diethy l-p-p he nylenediamine) to form a pink color which is proporti onal to the tota l bromine concent ration. The rang e of analysis is extended in the high range procedure by adding additional powder to increase the ratio of indicator to sample.
Replacement Parts (LR and HR)
Required Reagents
Description Unit Cat. No.
DPD Total Chlorine Reagent Po wder Pillows............................100/pkg.....21056-69
or
DPD Total Chlorine Reagent AccuVac
®
Ampuls..........................25/pkg.....25030-25
Page 36
1—36
Bromine, Total, HR, continued
Required Apparatus (Using AccuVac® Ampuls)
Description Unit Cat. No.
Beaker, 50 mL ......................................................................................each ......500-41H
Optional Reagents
Chlorine Standard Solution, Voluette® Ampules,
50-75 mg/L, 10 mL..................................................................... 16/pkg ....14268-10
Chlorine Standard Solution, Pour Rite Ampules,
25-30 mg/L.................................................................................. 20/pkg ....26300-20
Potassium Iodide Solution, 30 g/L.....................................100 mL MDB........ 343-32
Sodium Arsenite Solution, 5 g/L........................................100 mL MDB.......1047-32
Sodium Hydroxide Standard Solution, 1 N......................100 mL MDB .......1045-32
Sulfuric Acid Standard Solution, 1 N................................100 mL MDB .......1270-32
SwifTest™ Dispenser with DPD Total Reagent.................................each ....28024-00
Water, deionized....................................................................................4 L ........ 272-56
Optional Apparatus
AccuVac® Snapper Kit.......................................... ....... ........................each ....24 05 2-0 0
Caps for 10-mL sample cells............................................ ............. 12/pkg .... 24018-12
Caps for 1-cm/10-mL sample cells............................ ...... ....... ...........each ....5262 6-0 0
Page 37
1—37
Bromine, Total, HR, continued
Optional Apparatus, continued
Description Unit Cat. No.
Cylinder, graduated, 25 mL, poly........................................... ....... ....each.......1081-40
Cylinder, graduated, 100 mL, PMP........................................ ...........each.......2172-42
sens
ion™1 Basic Portable pH Meter, with electrode.....................each..... 51700-10
Pipet, TenSette
®
, 0.1 to 1.0 mL..........................................................each.....19700-01
Pipet Tips, For 19700-01 TenSette
®
..............................................50/pkg.....21856-96
Sample Cells, 10-mL with screw caps ............................................6/pkg.....24276-06
Replacement Parts
Batteries, AAA, alkaline...................................................................4/pkg.....46743-00
Instrument Cap/light shield............................................. ....... ....... ....each.....59548-00
Instruction Manual.............................................................................each.....59571-88
Sample Cells, 1-cm/10-mL........................... ....................................2/pkg.....41658-02
Page 38
1—38
Page 39
1—39
Chlorine, Free and T otal, HR (0.1 to 10.0 mg/L Cl
2
)
Method 10069 (Free)
For water, treated water, estuary water, and seawater
Method 10070 (Total)
For water, treated waters, wastewater, estuary water, and seawater
DPD Method*
USEPA accepted for reporting drinking water analyses (free and total chlorine) and wastewater analyses (total chlorine)
Measuring Hints
If the chlorine concentration is typically less than 2 mg/L, use the Chlorine Pocket Colorimeter (Cat. No. 58700-00).
Analyze samples immediately. Do not use plastic containers to collect samples. For best results, dedicate a set of cells to each test (free and total).
* Adapted from Standard Methods for the Examination of Water and Wastewater.
Page 40
1—40
Chlorine, Free and Total, HR, continued
High range free chlorine determinations are subject to variable levels of interferences from monochloramine. See Interferences on page 1—46.
Note: The Pocket Colo rimeter™ II is designed to measure solutions contained in sample cells.
DO NOT dip the meter in the sample or pour the sample directly into the cell holder.
Page 41
1—41
Chlorine, Free and T otal, HR, continued
1.Fill a 1-cm/10 -mL cell to
the 5-mL line with sample (the blank). Cap.
Note: Samples must be
analyzed immediately and cannot be preserved for later analysis.
2.Press the POWER key to
turn the meter on. The arrow should indicate
the chlorine channel (mg/L Cl
2
).
Note: See page 2—4 for
information on selecting the correct range channel.
3.Remove the meter cap.
Place the blank into the cell holder, with the diamond mark facing the back of the cell holder. Cover the cell with the cap.
Note: Wipe liq uid off sample
cells.
Page 42
1—42
Chlorine, Free and Total, HR, continued
4.Press: ZERO/SCROLL
The display will show “- - - -” followed by “0.0”.
Remove the blank.
5.Fill another 1-cm/10-mL
sample cell to the 5-mL line with sample. Cap.
Note: Do not use the same
sample cells for free and total chlorine without thoroughly rinsing the cells between the free and total tests.
6.Add the contents of one
DPD Free Chlorine or one DPD Total Chlorine Powder Pillows to the sample cell (the prepared sample). Cap the cell and shake gently for 20 seconds.
Note: Wipe liq uid off sample
cells.
Page 43
1—43
Chlorine, Free and T otal, HR, continued
7.For free chlorine, place
the prepared sample cell in the cell holder within one minute after adding the DPD Free Pillow. Cover the cell with the instrument cap. Proceed to step 9.
8.For total chlorine, plac e
the prepared sample in the cell holder and cover with the instrument cap. Wait three to six minutes after adding the DPD Total Pillows.Proceed to step 9.
9.Press READ/ENTER.
The instrument will show “- - - -” followed by the results in mg/L chlorine (Cl
2
).
Note: If the sample temporarily turns yellow after reagent addition or shows overrange
(page 2—12), dilute a fresh sample and repeat the test. A slight loss of chlorine may occur. Multiply the result by the dilution factor.
Page 44
1—44
Chlorine, Free and Total, HR, continued Accuracy Check
Standard Additions Method
a. Snap the neck off a high range Chlorine Standard Solution Voluette® Ampule,
50–70 mg/L Cl
2
.
b. Use a T enSette
®
pipet to add 0.1, 0.2, and 0.3 mL of standard to three separate
5-mL samples. Swirl gently to mix.
c. Analyze each sample as described in the procedure. Each 0.1 mL of standard
will cause an incremental increase in chlorine. The exact value depends on the concentration of the Voluette ampule standard. Check the certificate enclosed with the Voluette ampules for calculation of the expected increase in the chlorine concentration.
Standard Solution Method
Standard solutions for chlorine are difficult and time-consuming to prepare. Errors can occur if attention to detail is not addressed during preparation of the standards. The calibration curve is prepared under rigorous analytical laboratory conditions. Use the factory calibration fo r most normal testing.
Page 45
1—45
Chlorine, Free and T otal, HR, continued
A user calibration or a user-prepared chlorine standard may be required by a regulatory official or agency. Two options are available on the Pocket Colorimeter II to meet this requirement.
A chlorine standard may be prepared and used to validate the calibration curve using the Standard Calibration Adjust feature (see page 2—13 for more information). The concentration of the prepared standard must be determined with an alternate instrument such as a spectrophotometer, colorimeter, or by using an alternate method such as amperometric titration. The concentration of the chlorine standard for the HR procedure must be between 4.5 and 7.0 mg/L chlorine.
In addition, a user-generated calibration curve can be pr ogrammed into the Pocket Colorimeter II. See User-Entered Calibration on page 2—15 for more information.
Page 46
1—46
Chlorine, Free and Total, HR, continued Interferences
Interfering Substance
Interference Levels and Treatments
Acidity Greater than 150 mg/L CaCO3. May not develop full color or
color may fade instantly. Neutralize to pH 6–7 with 1 N Sodium Hydroxide. Determine amount to be added on separate 5-mL sample, then add the same amount to the sample being tested. Correct for the additional volume.
Alkalinity Greater than 250 mg/L CaCO
3
. May not develop full color or color may fade instantly. Neutralize to pH 6–7 with 1 N Sulfuric Acid. Determine amount to be added on separate 5-mL sample, then add the same amount to the sample being tested. Correct for the additional volume.
Bromine, Br
2
Interferes at all levels
Hardness No effect at less than 1,000 mg/L as CaCO
3
Iodine, I
2
Interferes at all levels
Page 47
1—47
Chlorine, Free and T otal, HR, continued
Manganese, Oxidized (Mn
4+
, Mn7+) or Chromium, Oxidized (Cr
6+
)
1. Adjust sample pH to 6–7.
2. Add 3 drops Potassium Iodide (30-g/L) (Cat. No. 343-32)
to a 5-mL sample.
3. Mix and wait one minute.
4. Add 3 drops Sodium Arsenite (5-g/L) (Cat. No. 1047-32)
and mix.
5. Analyze 5 mL of the treated sample as described in
the procedure.
6. Subtract the result from this test from the original analysis
to obtain the correct chlorine concentration.
Interfering Substance
Interference Levels and Treatments
Page 48
1—48
Chlorine, Free and Total, HR, continued
Monochloramine For conventional free chlorine disinfection (beyond the
breakpoint), monochloramine concentrations are very low. If monochloramine is present in the sample, its interference in the free chlorine test varies with the temperature, the relative amount of monochloramine to free chlorine, and the time required to do the analysis. Approximate interference levels of monochloramine in the free chlorine test are listed below (as mg/L Cl
2
).
Ozone Interferes at all levels.
Interfering Substance
Interference Levels and Treatments
NH2Cl Sample Temperatu re °C (°F)
(as Cl2) 5 (40) 10 (50) 20 (68) 30 (83)
1.2 0.2 0.2 0.3 0.3
2.5 0.4 0.5 0.6 0.6
3.5 0.5 0.6 0.7 0.8
Page 49
1—49
Chlorine, Free and T otal, HR, continued
Spec Secondary Standards
The DPD Chlorine Secondary Standards kit (Cat. No. 26353-00) cannot be used on the high range (HR) chlorine channel.
Method Performance
Estimated Detection Limit (EDL) = 0.1 mg/L Cl
2
Typical Precision (95% confidence interval) = 5.0 ± 0.2 mg/L Cl
2
Summary of Method
Chlorine can be present in water as free chlorine and as combined chlorine. Both forms can coexist in the same solution and can be determined together as total chlorine. Free chlorine is present as hypochlorous acid or hypochlorite ion. Combined chlorine represents a combination of chlorine-containing compounds including but not limited to monochloramine, dichloramine, nitrogen trichloride, and other chloro derivatives. The combined chlorine oxidizes triiodide ion (I
3
) to iodine (I2). The iodine and free chlorine reacts with DPD (N,N-diethyl-p-phenylenediamine) to form a red solution. The color intensity is proportional to the total chlorine concentration. To determine the concentration of combined chlorine, run a free chlorine test and a total chlorine test.
Page 50
1—50
Chlorine, Free and Total, HR, continued
Subtract the results of the free chlorine test from the total chlorine test to obtain the combined chlorine concentration.
The range of analysis using the DPD method for chlorine is extended by adding more indicator in proportion to sample volume. Thus, a larger, 25-mL size powder pillow of DPD Reagent is added to a 5-mL sample.
Replacement Parts
Required Reagents
Description U nit C at. No.
Free Chlorine Tests
DPD Free Chlorine Reagent
Powder Pillows for 25-mL sample...........................................100/pkg..... 14070-99
Total Chlorine Tests
DPD Total Chlorine Reagent
Powder Pillows for 25-mL sample...........................................100/pkg..... 14064-99
Page 51
1—51
Chlorine, Free and T otal, HR, continued
Optional Reagents
Description Unit Cat. No.
Chlorine Standard Solution, Voluette Ampules,
50–75 mg/L, 2-mL.....................................................................20/pkg..... 14268-20
Potassium Iodide Solution, 30 g/L ...................................100 mL MDB*......... 343-32
Sodium Arsenite Solution, 5 g/L........................ ................100 mL MDB....... 1047-32
Sodium Hydroxide Standard Solution, 1 N........................100 mL MDB....... 1045-32
Sulfuric Acid Stan d a rd Solution, 1 N.................................100 mL MDB....... 1270-32
Water, deionized ..................................................................................4 L......... 272-56
Optional Apparatus
AccuVac® Snapper Kit......................................................................each..... 24052-00
Batteries, AAA, alkaline.......................... ........................................4/pkg..... 46743-00
Caps for 10-mL sample cells.........................................................12/pkg..... 24018-12
Cylinder, graduated, 25 mL. glass.....................................................each......... 508-40
Cylinder, graduated, 100 mL, glass...................................................each......... 508-4 2
sens
ion1 Basic Portable pH Meter, with electrode......................each..... 51700-10
* Marked Dropper Bottle
Page 52
1—52
Chlorine, Free and Total, HR, continued
Optional Apparatus, continued
Description U nit C at. No.
Pipet, TenSette®, 0.1 to 1.0 mL......................................................... each..... 19700-01
Pipet Tips, For 19700-01 TenSette
®
Pipet.....................................50/pkg..... 21856-96
Replacement Parts
Cap for 1-cm/10 mL sample cell.......................................................each..... 52626-00
Instrument Cap/light shield................................................................each..... 59548-00
Instruction Manual.............................................................................each..... 59571-88
Sample Cells, 1-cm/10-mL............... .................................. .............2/pkg..... 48643-02
Page 53
1—53
Chlorine Dioxide (0.05 to 5.00 mg/L ClO
2
)
Method 10126
For water and wastewater
DPD Method* USEPA accepted for drinking water **
Measuring Hints
Chlorine dioxide samples cannot be stored, they must be analyzed immediately
after collection to minimize loss of chlorine dioxide.
Do not use plastic sample containers or measurement apparatus.
If the chlorine dioxide concentration exceeds the upper limit of the test (5.00 mg/L
ClO
2
), the color will not develop properly. The display will show overrange
(flashing 5.50) when the concentration is 5.50 or more. If the reading is over 5.00, dilute the sample with high quality water that is chlorine demand-free and repeat the test. Some loss of chlorine dioxide may occur during dilution. Multiply the result by the appropriate dilution factor.
* Adapted from Standard Methods for Examination of Water and Wastewater. ** Procedure is equivalent to Standard Methods, 4500 ClO
2
D.
Page 54
1—54
Chlorine Dioxide, continued
Use a timer for reagent reaction and be consistent for all samples.
Gently swirl samples to mix reagent s. Do not shake sample cells or ampules. Do not invert sample cells. AccuVac Ampuls can be inverted as they contain little air. Vigorous agitation may cause loss of volatile chlorine dioxide before it can react.
Allow any unreacted reagent to settle before taking readings.
For best accuracy when using AccuVac Ampuls, draw sample into an empty AccuVac ampule (Cat. No. 26779-25) and use that for the zero instead of a 10-mL sample cell.
Check the reagent blank for each new lot and at least every two months. Make this adjustment by using deionized water in the procedure instead of sample and subtract that reading from future test results.
Note: The Pocket Colo rimeter™ II is designed to measure solutions contained in sample cells.
DO NOT dip the meter in the sample or pour the sample directly into the cell holder.
Page 55
1—55
Chlorine Dioxide, continued
Chlorine Dioxide (using Powder Pillows)
1.Fill a 10-mL sample cell
with sample (the blank). Note: Samples must be
analyzed immediately.
2.Press the POWER key to
turn the meter on. The arrow should indicate
channel 1. Note: See page 2—4 for
information on selecting the correct range channel.
3.Place the cell into the cell
holder. Cover the cell with the instrument cap.
Page 56
1—56
Chlorine Dioxide, continued
4.Press ZERO/SCROLL.
The display will show “- - - -” then “0.00”.
Remove the blank from the cell holder.
5.Fill a second sample cell
with 10 mL of sample. Immediately add four drops of Glycine Reagent to the sample cell and swirl to mix.
6.Immediately add the
contents of one DPD Free Powder Pillow. Cap and swirl gently for 20 sec. Wait 30 sec. for undissolved powder to settle. Accuracy is not affected by undissolved powder.
Note: A pink color will
develop if ClO
2
is present.
Page 57
1—57
Chlorine Dioxide, continued
7.Within one minute of
adding the DPD to the sample, place the prepared sample into the cell holder.
8.Cover the sample with
the instrument cap.
9.Press READ/ENTER.
The display will show “- - - -”, followed by results in mg/L ClO
2
.
Page 58
1—58
Chlorine Dioxide, continued
Chlorine Dioxide (using AccuVac® Ampuls)
1.Fill a 10-mL sample cell
with sample (the blank). Note: Samples must be
analyzed immediately.
2.Press the POWER key to
turn the meter on. The arrow should indicate
channel 2. Note: See page 2—4 for
information on selecting the correct range channel.
3.Place the cell into the cell
holder. Cover the cell with the instrument cap.
Page 59
1—59
Chlorine Dioxide, continued
4.Press ZERO/SCROLL.
The display will show “- - - -” then “0.00”.
Remove the blank from the cell holder.
5.Collect 40 mL of sample
in a 50- or 100-mL beaker. Add 16 drops of Glycine Reagent to the 40 mL of sample. Swirl gently to mi x. Continue with step 6 immediately.
6.Fill a DPD Free Chlorin e
Reagent AccuVac Ampul with the pretreated sample in the beaker.
Note: Keep the tip immersed
until the ampule fills completely.
Page 60
1—60
Chlorine Dioxide, continued
7.Quickly invert the
ampule several times to mi x. Wait 30 seconds for any undissolved powder to settle. Accuracy is not affected by undissolved powder.
Note: A pink color will form
if chlorine dioxide is present.
8.Within one minute after
filling the ampule, place it into the cell holder. Cover the ampule with the instrument cap.
9.Press READ/ENTER.
The display will show “- - - -” followed by the results in mg/L chlorine dioxide.
Page 61
1—61
Chlorine Dioxide, continued
Sampling and Storage
Analyze samples for chlorine dioxide immediately after collection. Chlorine dioxide is a strong oxidizing agent and is unstable in natural waters. It reacts rapidly with various inorganic compounds, but oxidizes organic compounds more slowly. Many factors, including reactant concentrations, sunlight, pH, temperature, and salinity influence decomposition of chlorine dioxide in water.
Do not use plastic containers to collect samples for analysis since they often have a high chlorine dioxide demand. Pretreat glass sample containers to remove any chlorine or chlorine dioxide demand by soaking in a dilute bleach solution (1 mL commercial bleach to l liter of deionized water) for at least one hour. Rinse thoroughly with deionized or distilled water. If sample containers are rinsed thoroughly with deionized or distilled water after each use, only occasional pretreatment is necessary thereafter.
Failure to obtain a representative sample is a common error in testing for chlorine dioxide. If sampling from a tap, let the water flow for at least 5 minutes to ensure a representative sample. Let the container overflow with the sample several times, then cap the sample containers so there is no headspace (air) above the sample. If sampling with a sample cell, rinse the cell several times with the sample, then carefully fill to the 10-mL mark. Perform the chlorine dioxide analysis immediately.
Accuracy Check
Page 62
1—62
Chlorine Dioxide, continued
Because chlorine dioxide is difficult and hazardous to produce, check the DPD and Glycine Reagents by using chlorine standards. Proceed as follows:
1. Prepare a 1-mg/L free chlorine standard. a. Obtain Free Chlorine Standards (Cat. No. 14268-10). b. Determine the concentration of the standard from the certificate of analysis
shipped with the standard (50–75 mg/L Cl
2
). Calculate the volume of standard
needed as follows: mL standard needed = 100
÷ standard concentration
c. Pipet the volume of standard needed into a 100-mL volumetric flask. Dilute to
the line with chlorine demand-free deionized water. Invert to mix.
2. Perform the chlorine dioxide test on the standard without adding Glycine Reagent (step 3 of the procedures).
3. The chlorine dioxide reading should be 2.4 times greater than the chlorine concentration. If so, this verifies that the DPD Reagent and the instrument are working properly.
Page 63
1—63
Chlorine Dioxide, continued
4. Repeat the chlorine dioxide test on the chlorine standard, including the Glycine
addition. The reading should be less than 0.10 mg/L ClO
2
. This verifies that the
Glycine is eliminating free chlorine interference.
Standard Solution Method
Standard solutions for chlorine dioxide are difficult and time-consuming to prepare. Errors can occur if attention to detail is not addressed during preparation of the standards. Hach prepares the calibration curve under rigorous analytical laboratory conditions. Hach recommends using the factory calibration.
A user calibration or a user-prepared chlorine dioxide standard may be required by a regulatory official or agency . T wo options are available on the Pocket Colorimeter II to meet this requirement.
A chlorine dioxide standard may be prepared and used to validate the calibration curve using the Standard Calibration Adjust feature (see Standard Calibration Adjust on
page 2—13). The concentration of the prepared standard must be determined with an
alternate instrument such as a spectrophotometer, colorimeter, amperometric titration or by using another alternate method. The concentration of the chlorine dioxide standard must be between 2.00 and 4. 50 mg /L ch lorine dioxide.
Page 64
1—64
Chlorine Dioxide, continued
In addition, a user-generated calibration curve can be made and programmed into the Pocket Colorimeter™ II. See User-Entered Calibration on page 2—15.
Method Performance
Typical Precision (95% confidence interval):
4.78 ± 0.22 mg/L ClO
2
(AccuVac)
2.08 ± 0.04 mg/L ClO
2
(Powder Pillows)
Estimated Detection Limit:
EDL = 0.04 mg/L ClO
2
(AccuVac and Powder Pillows)
Interferences
Samples containing more than 250 mg/L alkalinity or 150 mg/L acidity as CaCO3 may inhibit full color development, or the color may fade instan tly. Neutralize these samples to pH 6–7 with 1 N Sulfuric Acid Standard Solution or 1 N Sodium Hydroxide Standard Solution. Determine the amount required on a separate 10-mL sample. Add the same amount to the sample to be tested. Correct for the additional volume.
Page 65
1—65
Chlorine Dioxide, continued
Samples containing monochloramine will cause a gradual drift to higher chlorine dioxide readings. When read within one minute of reagent addition, 3.0 mg/L monochloramine will cause an increase of less than 0.10 mg/L in the chlorine dioxide reading.
Bromine, chlorine, iodine, ozone and oxidized forms of manganese and chromium also interfere and read as chlorine dioxide.
T o compensate for the effects of manganese (Mn
4+
) or chromium (Cr6+), adjust the pH to 6–7 as described above. T o a 25-mL sample, add 3 drops of 30 g/L Potassium Iodide Solution, mix, and wait one minute. Add 3 drops of 5 g/L Sodium Arsenite Solution and mix. Subtract the result of this test from the original analysis to obtain the accurate chlorine dioxide concentration.
DPD Free Chlorine Reagent Powder Pillows and AccuVac Ampuls contain a buffer formulation that withstands high levels (at least 1000 m g/L) of hardness without interference.
Organic chloramines and peroxides may interfere. Various metals may interfere by combining with the Glycine Reagent needed to remove the chlorine interference. Metal interference is limited except when chlorine is present. In the presence of 0.60 mg/L Cl
2
, both copper (> 10 mg/L) and nickel (> 50 mg/L) interfere. Other metals may
Page 66
1—66
Chlorine Dioxide, continued
also interfere depending on their ability to prevent Glycine from reacting with any chlorine in the sample. It may be necessary to add more Glycine to overcome this interference.
Summary of Method
Twenty percent of the chlorine in the chlorine dioxide is reduced to chlorite, which reacts with DPD (N,N-diethyl-p-phenylenediamine) indicator to form a pink color. The color intensity is proportional to the ClO
2
in the sample. Chlorine interference is eliminated by adding Glycine Reagent, which converts free chlorine to chloroaminoascorbic acid, but has no effect on chlorine dioxide at the test pH.
Reagents and Apparatus
Required Reagents (Using Powder Pillows)
Description Units Cat. No.
ClO2 DPD Powder Pillow/Glycine Reagent Set (100 tests)..................... ..... 27709-00
Includes: (1) DPD Free Chlorine Reagent Powder Pillows, 100/pkg (1) Glycine Reagent, 29 mL
Page 67
1—67
Chlorine Dioxide, continued
Required Reagents (Using AccuVac Ampuls)
Description Units Cat. No.
ClO2 DPD AccuVac®/Glycine Reagent Set (25 tests)............................ . ..... 27710-00
Includes: (1) DPD Free Chlorine Reagent AccuVac
®
Ampuls, 25/pkg
(1) Glycine Reagent, 29 mL
Require Apparatus (Using AccuVac Ampuls)
Beaker, 50-mL, glass.........................................................................each......... 500-41
Beaker, 100-mL, glass.......................................................................each......... 500-42
Optional Reagents
AccuVac® Ampuls for Blanks.......................................................25/pkg..... 2 6779-25
Chlorine Standard Solution Voluette™ Ampules,
50–75 mg/L, 10-mL...................................................................16/pkg..... 14268-10
Potassium Iodide Solution, 30 g/L ....................................100-mL MDB......... 343-32
Sodium Arsenite Solution, 5 g/L........................ ...............100-mL MDB....... 1047-32
Page 68
1—68
Chlorine Dioxide, continued
Optional Reagents, continued
Description Units Cat. No.
Sodium Hydroxide Standard Solution, 1 N.......................100-mL MDB....... 1045-32
Sulfuric Acid S tan dard Solution, 1 N........................... .....100-mL MDB....... 1270-32
Water, deionized ..................................................................................4 L.........272-56
Optional Apparatus
AccuVac® Snapper Kit......................................................................each..... 24052-00
Caps for 10-mL sample cells.........................................................12/pkg..... 24018-12
Cylinder, graduated, 25-mL, glass.....................................................each......... 508-40
Cylinder, graduated, 100-mL, glass...................................................each......... 508-42
sension™1 Basic Portable pH Meter, with electrode........................each..... 51700-10
Pipet, TenSette
®
, 0.1 to 1.0 mL......................................................... each..... 19700-01
Pipet Tips, for 19700-01 TenSette
®
Pipet......................................50/pkg..... 21856-96
Replacement Parts
Batteries, AAA, alkaline............................ ......................................4/pkg..... 46743-00
Instrument Cap/light shield................................................................each..... 59548-00
Instrument Manual.............................................................................each..... 59571-88
Sample Cell, 25 x 60 mm 10 mL mark............................................6/pkg..... 24276-06
Page 69
1—69
pH (6.0 to 8.5 pH units)
For water and wastewater
Method 1 0 076
Phenol Red Method
Measuring Hints
For greatest accuracy, use the Standard Calibration Adjust to adjust the
calibration curve with each new lot of Phenol Red. Use the pH 7.00 Buffer Solution included in the kit.
Periodically, recheck with the pH 7 Bu ffer to confirm the accuracy of the
instrument and method. If not rea ding within 0.1 pH unit, recalibrate th e instrument.
The amount of indicator a nd sample is critical for accurate results and sh ould
be measured carefully.
Attempting to measure a sample with a pH below 6.0 or above 8.2 will result
in an inaccurate reading. Measurements outside the range can differ from the true pH reading by as much as 2 pH units.
Note:
The Pocket Colorimeter II is designed to measure solutions contained in sample cells.
DO NOT
dip the meter in the sample or pour the sample directly into the cell holder.
Page 70
1—70
pH, continued
1.Collect about 50 mL of
sample in a beaker and fill a 10-mL sample cell to the 10-mL mar k with sample.
2.Pr ess the POWER key to
turn the meter on. The arrow sh ould indicate
pH.
Note:
See page 2—4 for information on selecting the correct range channel.
3.Using the calibrated
dropper, add 0.5 mL of Phenol Red Solution to the cell. Cap and invert to mix.
Note:
For greatest accuracy,
use a clean and dry dropper.
Page 71
1—71
pH, continued
4.Fill a second sample cell
to the 1 0-mL mark with the original sample. Cap the sample cell. This is the blank.
5.Place the blank into the
cell holder.
Note:
Wipe liquid off sample cells or damage to the instrument may occur.
6.Cover the cell with the
instrument cap.
Page 72
1—72
pH, continued
7.Press ZERO/SCROLL.
The display will show “- - - -” then “0.0”.
Remove the blank fro m the cell holder.
8.Place the prepared
sample in the cell holder.
Note:
Wipe liquid off sample
cells.
9.Cover the cell with the
instrument cap.
Page 73
1—73
pH, continued
10. Press READ/ENTER.
The display will show “- - - -”, followed by results in pH units.
Page 74
1—74
pH, continued Accuracy Check
Preparation of pH 7.0 Standard Solution
A pH 7.00 standard solution is necessary to calibrate or check the accuracy of the pH measurement using the Standard Calibration Adjust feature (see Standard Calibration
Adjust on page 2—13). Use the pH 7.00 Buffer Vial (in cluded in this kit) or bulk buffer
solution (see Optional Reagents on page 1—76). Add 0.5 mL of Phenol Red Solution to 10 mL of pH 7.00 Buffer Solution to prepare the color standard. Do not use col ored buffer solutions.
For greatest accuracy, adjust the calibration curve using Standard Calibration Adjust with each new lot of Phenol Red Indicator. Periodically check the strength of the indicator by testing a pH 7.0 Buffer Solution.
Method Performance
Typical Precision (95% CI):
7.0 ± 0.1 pH
Page 75
1—75
pH, continued
Standard Calibration Adjust
To perform a standard calibration adjustment using the pH 7.0 buffer, see Standard
Calibration Adjust on page 2—13.
Summary of Method
Proper pH control in drinking water and swimmin g po ols is necessary fo r m an y reasons. Bactericidal activity of chlorine is greatest when the pH is less than 7.4. Alum-type flocculents, important for clear water, perform best in a pH range of 7.2 to 8.0. Keeping the pH below 8.0 is important to control algae. A sudden rise in pH may signal an increase in algal growth. If the pH drops below 7.0, corrosion of pipes and metal fixtures may occur. Eye irritation is minimized when the pH is kept between 7.2 and 7.6.
Phenol Red is a phthalein indicator which has a transition window of pH 6.8 (yellow) to 8.2 (red). The pH is determined colorimetrically from the change in the absorbance of the alkaline peak.
Page 76
1—76
pH, continued Replacement Parts
Required Reagents
Description Unit Cat. No.
Buffer Solution, pH 7.0....................................................................25 mL ....12222-20
Phenol Red Solution, Spec-grade...................................................50 mL ....26575-12
Required Apparatus
Sample Cells, 10 mL, with caps.......................................................6/pkg ....2427 6-0 6
Optional Reagents
Buffer Solution, pH 7.0................................................................. 500 mL ....12222-49
Water, deionized................................................... ......................... 500 mL . ....... 272-49
Optional Apparatus
Droppers, 0.5 and 1.0 mL.............................................................. pkg/20 .... 21247-20
Replacement Parts
Batteries, AAA, alkaline ...................................................................4/pkg ....46743-00
Instrument Cap/light shield................... .............................................each ....59548-00
Instruction Manual.......................... ....... .............................................each ..... 5 95 71-88
Page 77
2—1
Section 2
Instrument Manual
Page 78
2—2
Page 79
2—3
Instrument Operation
Key Functions
Key Description Function
POWER On/Off/Backlight
To turn on the backlight, turn on the instrument, then press and hold the power key until the backlight turns on. Press and hold again to turn off the backlight. This key functions the same in all instrument modes and ranges.
ZERO/SCROLL In measurement mode, sets the instrument to zero.
In menu mode, scrolls through menu options. Also scrolls numbers when entering or editing a value.
READ/ENTER In measurement mode, initiates sample measurement.
In menu mode, selects a menu option. When entering numbers, moves one space to the right and executes the function when the entry is complete.
Page 80
2—4
Instrument Operation, continued
Menu Selections
Press the MENU key to access the menu selections.
Switching Ranges
1. Press the MENU key. The display will show “SEL”. A flashing arrow indicates the current range.
2. Press the
READ/ENTER key to toggle between ranges.
3. Press
MENU again to accept and exit back to the measurement screen.
Setting the Time
1. Press the MENU key, then press the ZERO/SCROLL key un til th e di sp lay shows a time in the “00:00” format.
MENU Enter/Exit the menu mode
Press and hold for approximately 5 seconds to enter user-entered method mode.
Key Description Function
Page 81
2—5
Instrument Operation, continued
2. Press READ/ENTER. The digit to be edited will flash.
3. Use the
ZERO/SCROLL key to change the entry, then press READ/ENTER to
accept and advance to the next digit. The time is entered in 24-hour format.
Recalling Stored Measurements
1. Press the MENU key, then press the ZERO/SCROLL key until the display shows
RCL. The instrument automatically stores the last 10 measurements.
2. In RCL, press
READ/ENTER to recall the stored measurements, beginning with
the most recent measurement taken. The meter stores the measurement number as 0 1 (most recent) through 1 0 (oldest), the time the measurement was taken, and the measurement value. The
ZERO/SCROLL key allows for selection
of a specific measurement by number. The
READ/ENTER key scrolls through all
stored data points.
Page 82
2—6
Instrument Operation, continued
Battery Installation
Figure 1 on page 2—7 provides an exp lod ed vi ew of battery installation.
1. Unhook the latch and remove the bat tery co mpartment cover. The polarities are shown on the battery holder.
2. Place the four batteries provided with the instrument in the holder as indicated and replace the battery compartment cover. The display will show the software version number (e.g., “P 1.6”) after correct battery installation.
When replacing discharged batteries, always replace the complete set of four alkaline batteries. Rechargeable batteries are not recommended and cannot be recharged in the instrument.
Note:
The Low Battery icon will appear on the display when the batteries have 10 % battery life remaining. The battery icon will flash when the batteries are too low to complete measurements. See Instrument Keys and Display on page 1—11.
Page 83
2—7
Instrument Operation, continued
Figure 1 Battery Installation
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2—8
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2—9
Error Codes
When the instrument canno t perfo r m th e funct io n in it iat ed by the operator, an error message will appear in the display. Refer to the appropriate message information below to determine what the problem is and how it can be corrected. Resolve error messages in the order that they appear on the display. Service Centers are listed in page 2—37.
Error Messages
1. E-0 No Zero (User mode)
Error occurs when trying to read a standard in the user calibration mode before setting the meter to zero.
Zero the instrument on an appropriate blank.
2. E-1 Ambient Light Er ro r
There is too much light present to take a valid measurement.
Verify instrument cap is correctly seated.
If the problem persists, contact a Service Center (page 2—37).
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Error Codes, continued
3. E-2 LED Error
The LED (light source) is out of regulation.
Replace batteries.
Verify LED lights up (inside the cell holder) when the READ/ENTER or
ZERO/SCROLL key is pressed.
If the problem persists, contact a Service Center (page 2—37).
Note: When an E-1 or E-2 error occurs on a measurement, the display will show “_.__”. (The
decimal place is determined by the chemistry.) If the E-1 or E-2 error occurs while zeroing the meter , the meter will require the user to re-zero.
4. E-3 Standard Adjust Error
The value obtained on the prepared standard exceeds the adjustment limits allowed for the standard concentration, or the concentration of the standard is outside the concentration range allowed for standard calibration adjust.
Prepare the standard and rerun according to the procedure.
Prepare a standard at or near the recommended concentrations given in the
procedure.
Verify that the concentration of the standard has been entered correctly.
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Error Codes, continued
If the problem persists, contact a Service Center (page 2—37).
5. E-6 Abs Error (User mode )
Indicates that the absorbance value is invalid, or indicates an attempt to make a curve with less than two points.
Enter or measure the absorbance value again.
If the problem persists, contact a Service Center (page 2—37).
6. E-7 Standard Value Error (User mode)
Standard concentratio n is equ al to another standard concentr ati on tha t is already entered.
Enter the correct standard concentration.
If the problem persists, contact a Service Center (page 2—37).
7. E-9 Flash Error
The meter is unable to save data.
If the problem persists, contact a Service Center (page 2—37).
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Error Codes, continued
8. Underrange—flashing number below stated test range
Verify instrument cap is correctly seated.
Check zero by measuring a blank. If error recurs, re-zero the instrument.
If the problem persists, contact a Service Center (page 2—37).
Note: See Maximum/Minimum Displayed Value on page 2—26 for more information.
9. Overrange—flashing number above stated test range
Note: Flashing value will be 10% over the upper test limit.
Check for light blockage.
Dilute and retest sample.
Note: See Maximum/Minimum Displayed Value on page 2—26 for more information.
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Standard Calibration Adjust
The Pocket Colorimeter™ II instrument is factory-calibrated and ready for use without user calibration. Use of the factory calibration is recommended unless the user is required to generate a calibration. The Standard Calibration Adjust can be used to meet regulatory requirements.
This feature allows the factory default calibration curve to be adjusted with a known standard. Use the standard described in the procedure.
1. Place a blank in the meter (in measurem ent mo de). Press
ZERO/SCROLL.
2. Place the reacted standard in the meter. Press
READ/ENTER.
3. Press
MENU, then press ZERO/SCROLL until the display shows “SCA”.
4. Press
READ/ENTER to display the standa rd calibration adjust value.
5. Press
READ/ENTER to adjust the curve to the displayed value. The meter will
return to the measurement mode and the Calibration Adjusted icon will appear in the display window.
If an alternate concentration is used, or if a standard concentration is not given:
6. Repeat steps 1–4.
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Standard Calibration Adjust, continued
7. Press ZERO/SCROLL to access the Edit function, then press READ/ENTER to begin editing. The digit to be edited will flash. Use the
ZERO/SCROLL key to
change the entry, then press
READ/ENTER to accept and advance to the
next digit. When the last digit is entered, press
READ/ENTER and the meter will adjust the
curve to the value entered. The meter will return to measurement mode and the Calibration Adjusted icon will appear in the display window.
To turn off Standard Calibration Adjust (SCA):
1. Press
MENU.
2. Press
ZERO/SCROLL until “SCA” appears in the display.
3. Press
READ/ENTER, then press ZERO/SCROLL until “Off” appears in the display.
4. Press
READ/ENTER to turn off SCA.
Note: Perform another standard calibration adjust to turn SCA on again. Note: For meters with factory-calibrated ranges or methods, Standard Calibration Adjust
(SCA) will be disabled when a user-entered method is programmed into the meter. To turn SCA back on, restore the meter to factory default calibration. See Retrieving the Factory Calibration on page 2—25.
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User-Entered Calibration
Overview
The Pock et Colorimeter™ II will accept a user-prepared calibration curve. The curve can extend from 0 to 2.5 absorbance. A user-prepared calibration curve may be entered into any channel that does not contain a factory-progr ammed curve. These channels are labeled “abs” on instruments having a single factory calibration or are labeled “1” and “2” on the uncalibrated single wavelength instruments. Any chemistry that can be run at the instrument wavelength may be user-entered in these channels.
Using prepared standard solutions that cover the range of interest, th e mete r generates a calibration curve by calculatin g th e stra igh t-l in e segments between each standard entered. A calibration curve may be entered using the keypad. Factory-entered calibration curves may also be recalculated or adjusted using the same procedure.
To enter the user-entered calibration mode, press the
MENU key and hold it down
until the display shows “USER” (about 5 seconds), followed by “CAL”. Press
ZERO/SCROLL to scroll through the options.
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User-Entered Calibration, continued
CAL—Used to enter and edit standard values and measure absorbance values,
or review the existing calibration.
Edit—Used to enter and edit standard values and ab sorbance values with the
keypad or review the existing calibration. Used to enter a predetermined calibration curve.
dFL—Used to return the instrument back to the default factory calibration.
User-entered calibrations are stored upon exit from the calibration or edit modes.
Note: To return to factory settings, following the instructions in Retrieving the Factory
Calibration on page 2—25.
If the instrument is shut off or loses power during data entry, all edits will be lost. Automatic shut-off in user-entered cali br at io n entry mode is 60 minutes.
CAL and Edit Submenus
In CAL mode, standard values are entered and absorbance values are measured. In Edit mode, standard and absorbance values are entered.
To select CAL from the User menu, press READ/ENTER.
To sel ect Edit from the User menu, press ZERO/SCROLL and READ/ENTER.
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User-Entered Calibration, continued
Once in the CAL or Edit optio n, press the READ/ENTER key to navigate through
each option.
Note: Press
ZERO/SCROLL
to quickly scroll through each option.
Calibration Procedure Using Prepared Standards
Note:
Deionized water or a reagent blank can be used to zero during the calibration procedure. Calibrations generated with deionized water as the zero will give less accurate results if the reagent blank is significantly more turbid or colored than deionized water. Use the deionized water or the reagent blank as the zero concentration point (S0) in the following calibration procedure.
1. Turn on the instrument and select the range to be calibrated. An arrow at the top of the display will point to the selected range. To change ranges, press the
MENU key, then use the READ/ENTER key to toggle between ranges 1 and 2.
Press
MENU again to return to measurement mode.
2. Follow the procedure for the chemical method to be calibrated . Prepare a reagent blank (if needed) and a standard solution. Allow the color to develop fully.
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User-Entered Calibration, continued
3. Insert the reagent blank or deionized water into the meter and cover with the cap. Press the
ZERO/SCROLL key . Th e meter will displ ay “- - - -”, followed by
“0.000”. This initializes (zeroes) the meter.
4. Press the
MENU key and hold it down until the display shows “USER”, followed
by “CAL”. Press
READ/ENTER to enter the calibration mode.
5. In factory-calibrated meters, S0 will appear in the display.
Note: When recalibrating a factory-calibrated meter or range, RES (resolution) cannot
be changed.
6. In uncalibrated meters or meters with ranges labeled Abs, “RES” will appear. Press
ZERO/SCROLL to review the current resolution (decimal placement). Press
ZERO/SCROLL again to accept the current resolution. To change the resolution,
press
READ/ENTER, then ZERO/SCROLL to change the resolution. Press
READ/ENTER to accept the new resolution. “S0” will appear on the display.
7. Press the
READ/ENTER key again, then enter the blank value.
Note: Press the
READ/ENTER
key to move from digit to digit. Use the
ZERO/SCROLL
key to
change the number.
8. After completing entry of the blank value, press the READ/ENTER key. The display will show “A0”.
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User-Entered Calibration, continued
9. Insert the reagent blank or deionized water into the cell holder. Cover the
blank with the instrument cap.
10. Press the
READ/ENTER key . The meter will measure and display the absorbance
value for “S0”.
11. Remove the sample blank. Press the
ZERO/SCROLL key . “S1” will appear . Press
the
READ/ENTER key, then enter the first standard value.
Note: Press the
READ/ENTER
key to move from digit to digit. Use the
ZERO/SCROLL
key to
change the number.
12. After completing entry of the first standard value, press the READ/ENTER key.
The display will show “A1”.
13. Insert the first reacted standard solution into the cell holder. Cover the
prepared standard with the instrument cap.
14. Press the
READ/ENTER key . The meter will measure and display the absorbance
value for S1.
15. The calibration is complete with two points. If additional standards are
required, press
ZERO/SCROLL until “Add” appears on the display. Repeat
steps 1114 to enter additional standards.
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User-Entered Calibration, continued
16. Press the MENU key twice to exit and accept the changes. The instrument will use this calibration to determine the displayed concentration of future sample measurements.
Entering a Predetermined Calibration Curve
Note: Entering a predetermined calibration curve requires at least two data pairs. Each data
pair requires a concentration value and the absorbance value for the given concentration. Up to 10 data pairs may be entered. This procedure uses the Edit mode.
1. Turn on the instrument and select the range to be calibrated. An arrow at the top of the display will point to the selected range. To change ranges, press the
MENU key, then use the READ/ENTER key to toggle between ranges 1 and 2.
Press
MENU again to return to measurement mode.
2. Press the
MENU key and hold it down until the display shows “USER”, followed
by “CAL”. Press
ZERO/SCROLL to scroll to EDIT. Press READ/ENTER.
3. In uncalibrated meters or in Abs range, “RES” will appear. Press ZERO/SCROLL. To change the resolution (decimal placement), press
READ/ENTER. Press
ZERO/SCROLL to select the new resolution, then press READ/ENTER to accept.
“S0” will appear on the display.
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User-Entered Calibration, continued
4. Enter the concentration value and absorbance value of the first data pair
(S0, A0).
5. To enter the S0 value, press
READ/ENTER. Use the ZERO/SCROLL key to select
the numerical value, then press the
READ/ENTER key to accept the entry and
advance to the next decimal place. Repeat this sequence until the S0 concentration value is entered.
6. After editing the S0 value, press
READ/ENTER to accept. “A0” will appear on
the display.
7. To enter the absorbance value for S0, press the
READ/ENTER key to go to entry
mode. Use the
ZERO/SCROLL key to select the numerical value, then press the
READ/ENTER key to accept the entry and advance to the next decimal place.
Repeat this sequence until the absorbance value for S0 is entered.
8. After enterin g A0, press
READ/ENTER to accept. “S1” will appear on the
display.
9. Repeat steps 5 through 8 for each standard value and absorbance value pair in
the calibration curve
Note: After A1 is entered, Add will appear in the display. If additional data pairs are to be
entered, press
READ/ENTER
and continue with step 9.
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User-Entered Calibration, continued
10. When all the calibration data has been entered, press MENU twice to return to the measurement mode.
Editing a User-entered or Factory Calibration Curve
1. Press the MENU key and hold it down until the display shows “USER”, followed by “CAL”. Press
ZERO/SCROLL until EDIT appears.
2. Press the
READ/ENTER key to enter Edit mode. In factory-calibrated meters,
“S0” will appear in the display.
Note: When editing a factory-calibrated meter or range, RES (resolution) cannot be changed. Note: When RES or S0 appears in the display, press
ZERO/SCROLL
to quickly scroll to the
data to be edited.
3. In uncalibrated meters or in Abs range, “RES” will appear . Press ZERO/SCROLL to review the current resolution. Press
ZERO/SCROLL again to accept the
displayed resolution. To change the resolution (decimal placement), press
READ/ENTER. Press ZERO/SCROLL to select the new resolution, then press READ/ENTER to accept. “S0” will appear on the di splay.
4. Press
READ/ENTER. The current concentration value for S0 will appear on the
display.
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User-Entered Calibration, continued
5. To edit the S0 value, press READ/ENTER. Use the ZERO/SCROLL key to select the
numerical value, then press the
READ/ENTER key to accept the entry and
advance to the next decimal place. Repeat this sequence until the S0 concentration value is entered.
6. After editing the S0 value, press
READ/ENTER to accept. “A0” will appear on
the display.
7. To edit the absorbance value for S0, press th e
READ/ENTER key to go to entry
mode. Use the
ZERO/SCROLL key to select the numerical value, then press the
READ/ENTER key to accept the entry and advance to the next decimal place.
Repeat this sequence until the absorbance value for S0 is entered.
8. After editing A0, press
READ/ENTER to accept. “S1” will appear on the display .
9. Repeat steps 4 through 8 for each standard value and absorbance value pair in
the calibration curve.
10. When all calibration data has been reviewed or edited, “ADD” will appear in
the display.
11. Press
READ/ENTER to add more calibration points, or press MENU twice to
return to the measurement mode.
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User-Entered Calibration, continued
Note: When a factory calibration curve has been edited, the “calibration adjust” icon will
appear in the display.
Exiting the Calibration Routine
Exit the calibration routine by pressing th e MENU key to return to measurement mode. The instrument uses the last completed user-entered calibration or the factory calibration if no user-entered calibration has been completed.
Deleting Calibration Points
1. Select the range containing user-entered calibration points. See Switching
Ranges on page 2—4.
2. Press and hold the
MENU key until “USER”, then “CAL” appears. Press
READ/ENTER.
Note: Calibration points can also be deleted in Edit mode.
3. Press ZERO/SCROLL to select the point to delete (e.g., S0 or S1 or S2). Press
READ/ENTER.
4. The left digit will flash. Press
ZERO/SCROLL until “dEL” appears. (“dEL” will
appear after the numeral 9.)
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