Accuracy*: ± 1% for readings over 100 digits. (Uncertainty of
readings is 1 digit. Most samples require more than 100 digits.)
Weight: 132 g (4.7 oz.)
Cartridges for the Digital Titrator
Volume: 13 mL
Number of tests: Most reagents are formulated to provide 100
typical titrations; the number may vary depending on sample
concentration.
Weight (full): 56.75 g (2 oz.)
* Overall method accuracy includes, in addition to the Digital Titrator, other sources of error controlled
by the analyst. The other sources of error include: sampling, sample volume, dilution (if required), end
point detection, reagent quality, and interferences.
7
8
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 dangereuse. Lire 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 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 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.
9
10
GENERAL DESCRIPTION
1.1Introduction
Hach’s Digital Titrator is a new concept in titrimetric analysis. It
is a precision dispensing device fitted with compact cartridges
that contain concentrated titrants. Accurate titrations are made
without the bulk and fragility of conventional burets.
A main drive screw in the Digital Titrator controls a plunger
which forces the concentrated titrant from a titration cartridge in a
carefully regulated flow. The titrator body is constructed of
precision-molded, heavy-duty, chemical- and impact-resistant
acetal plastic. Accuracy is rated at ± 1% or better for a titration of
more than 100 digits. For titrations less than 100, accuracy is ± 1
digit.
Titration solutions (titrants) are packaged in disposable
polypropylene or Kynar
neoprene seals and polyethylene resealable closures to cover the
cartridge tips. Each cartridge contains approximately 13 mL of
titrating solution, enough for 50–100 average titrations. Titrant
solutions are typically controlled to ± 0.5% concentration with
normality and tolerances listed on the label. Titrant
concentrations are designed for titrations of 10 to 40 turns
(100 to 400 digits) of the delivery knob. For the most commonly
used concentration ranges, the digits appearing in the counter
window correspond to the sample concentration.
®
containers with Teflon-covered
Figure 1Hach Digital Titrator
11
GENERAL DESCRIPTION, continued
Both portable and fixed-position titrations are possible with the
Digital Titrator. The instrument has a grip for hand-held operation
or it can be clamped to a TitraStir
for stationary setups. See Figure 1.
Each Digital Titrator comes with five delivery tubes and a
methods manual, which covers the most commonly tested
parameters and the corresponding titrant cartridges. Right-angle
(ninety-degree) delivery tubes for stationary setups are available
as an optional accessory.
1.1.1Following a Procedure for the First Time
Each method is divided into five sections: Procedure, Accuracy
Check, Interferences, Summary of Method, and Reagents and
Apparatus. For more information about how to select a procedure
or for answers to chemical questions, see Hach’s Water Analysis Handbook (literature 8376). For more information about chlorine
measurement, also see the technical booklet titled, Current Technology of Chlorine Analysis for Water and Wastewater
(literature 7019).
The Procedure details how to perform the method step-by-step.
To select the appropriate sample volume and titration cartridge
based on expected sample concentration, use the tables provided
in each procedure. If the expected sample concentration is not
known, start with one of the smaller sample volumes and
determine its approximate concentration. Retest with the
appropriate sample size.
®
Stir Plate or laboratory stand
The ranges in the table overlap to offer more flexibility. In most
procedures, the number of digits used for each concentration
range will be 100 to 400 digits.
To determine the actual concentration of the sample, use the
correct digit multiplier for the sample volume and titration
cartridge used.
Throughout the procedure, the notes will provide
additional information.
The Accuracy Check provides a way to verify the results and
determine if interferences are present. It also provides a method
for checking the performance of reagents, the Digital Titrator and
the operator’s technique. Further information is provided in
Appendix A, Accuracy Check and Standard Additions.
12
GENERAL DESCRIPTION, continued
The Interferences section identifies common interferences
causing inaccurate results and describes how to eliminate their
effects. The interference levels are based on the sample volume
that has 1.0 as the digit multiplier. Higher interference levels may
be tolerated if a smaller sample is used.
The Summary of Method section discusses the chemical
reaction taking place and information that applies to the
entire procedure.
The Reagents and Apparatus list concludes the procedure. All
the items required to perform the test are listed first and are
available from Hach. The items listed in the notes or interferences
sections are included in the optional listings.
1.2Step-By-Step
1. Select a sample volume and titration cartridge corresponding
to the expected sample concentration from the table given in
each procedure.
If the expected sample concentration is not known, start with
one of the smaller sample volumes and determine its
approximate concentration. Retest with the appropriate
sample size.
2. Slide the cartridge into the titrator receptacle and lock in
position with a slight turn. See Figure 2.
Figure 2Sliding the Cartridge into Place
3. Remove the polyethylene cap and insert a clean delivery tube
into the end of the cartridge until it is tight. See Figure 3. Use
a straight tube with a hook at the end for hand-held titrations;
use a 90° tube with a hook at the end for stationary setups.
13
GENERAL DESCRIPTION, continued
Do not insert tube past cartridge extension; see illustration
below. In some instances, it might be necessary to remove a
small burr on the leading edge of the tube before insertion.
Figure 3Inserting the Delivery Tube
4. For stationary titrations, use a TitraStir Stir Plate or a clamp
holder and clamp to attach the titrator to a laboratory stand.
See Figure 4 and Figure 5.
The TitraStir Stir Plate holds the Digital Titrator during the
titration and also stirs the sample at a constant speed, leaving
the analyst free to detect the end point. When a TitraStir Stir
Plate is used, substitute or add the following
Optional Apparatus.
APPARATUS
Quantity Required
DescriptionPer TestUnitCat. No.
Delivery Tubes, 90° with hook for TitraStir® Stir Plate........... 1 ............. 5/pkg .......... 41578-00
Flask, Erlenmeyer, 125 mL....................................................... 1 ............... each .............. 505-43
Flask, Erlenmeyer, 250 mL....................................................... 1 ............... each .............. 505-46
Stir Bar, 28.6 x 7.9 mm............................................................. 1 ...............each.......... 20953-52
TitraStir
TitraStir
®
Stir Plate, 115 Vac....................................................1 ............... each .......... 19400-00
®
Stir Plate, 230 Vac....................................................1 ............... each .......... 19400-10
5. To start titrant flowing and flush the delivery tube, hold the
tip of the cartridge up. Advance the plunger release button to
engage the piston with the cartridge (push the button in and
toward the cartridge). Do not expel solution when pushing the
piston toward the cartridge. Turn the delivery knob until air is
expelled and several drops of solution flow from the tip. As
you turn the knob a drive screw pushes a piston against the
cartridge seal and forces liquid out through the delivery tube.
Then use the counter reset knob to turn the digital counter
back to zero and wipe the tip. The tip can be rinsed with
deionized water rather than wiped, if desired.
14
GENERAL DESCRIPTION, continued
Figure 4Using the TitraStir® Stir Plate
Figure 5Using a Laboratory Stand
15
GENERAL DESCRIPTION, continued
Figure 6Titrating the Sample
6. Use the smallest appropriate graduated cylinder or pipet to
measure the sample volume from the given table. Transfer the
sample into a 125-mL or 250-mL Erlenmeyer flask. Dilute to
the appropriate total volume with deionized water
if necessary.
Note: Sample volume measurements and dilutions (if required) must be
made accurately. However, final total volume of titrated solution is
not critical.
7. Add the necessary reagents to the sample and swirl to mix.
8. Immerse the delivery tube tip in the solution and swirl the
flask while titrating. Titrate by turning the delivery knob.
Keep turning the knob and swirling the sample until the end
point is reached. Record the number of digits that appear in
the digital counter window. See Figure 6.
16
GENERAL DESCRIPTION, continued
Note: The number of digits required will usually range from 100 to 400.
In nearly all of the procedures if the digits required is less than 100
or more than 400, an alternate sample volume or titrant cartridge
should be used.
Note: Inaccurate results will occur if the delivery tube tip is held out of
the solution rather than under the solution surface.
9. Calculate the concentration of your sample by using the
Digits Required = the number that appeared in the digital counter
window in Step 8.
Digit Multiplier = the number from the table given in the procedure.
It takes into account the sample dilution and titrant strength.
10. After completing testing for the day, press the plunger release
button and manually retract the plunger into the body of the
titrator. Remove the cartridge. Remove the delivery tube and
reseal the cartridge with the polyethylene cap. See Figure 7.
Figure 7Retracting the Plunger
11. Discard or clean the delivery tube immediately after use. To
clean, force water, then air, into the tube opening with a
syringe or wash bottle.
17
GENERAL DESCRIPTION, continued
1.3Helpful Hints
1.3.1To Reuse a Partially Emptied Cartridge
1. With the plunger fully retracted, attach cartridge to
the titrator.
2. Press the plunger release; then manually push the plunger
against the cartridge seal.
3. Attach a delivery tube. Hold the tip of the cartridge up. Eject
air and a few drops of titrant, zero the counter, and wipe
the tip.
4. Titrate as usual.
1.3.2To Calculate Titrant Volume Used
Normalities of many Hach titration cartridge solutions have been
designed so that the number of digits used in a titration
corresponds to the sample concentration in mg/L. To determine
the volume used in mL, divide the Digital Titrator reading by 800.
1.3.3To Fill Your Own Titration Cartridges
Cartridges may be cleaned and refilled, or new empty cartridges,
Cat. No. 14495-01, can be purchased from Hach Company. See
Figure 8. When preparing to refill old cartridges, push the
cartridge seal out of the cartridge with air pressure applied
through the tip. Cap the tip, fill with solution and reinsert the
cartridge seal using care to avoid wrinkling the Teflon sheath.
Filling also can be accomplished at the tip with a syringe.
Figure 8Digital Titrator Cartridges
18
GENERAL DESCRIPTION, continued
1.3.4Verifying Technique
Whenever procedures are changed or new equipment is used, it is
helpful to run a sample of known concentration. This technique
will confirm the operator is following the procedure correctly and
the new equipment is working properly. One objective important
to Hach Company is making our tests self-verifying. This means
Hach makes the tools available so the operator can check their
own work for accurate results without relying on an outside lab
or chemist.
For most of the tests in this manual, Table 1 on page 20 lists each
procedure, the suggested standard, the volume of standard
needed, the titration cartridge used, and the number of expected
digits when the test is performed correctly. The suggested
standards are Voluette
possible because of their superior accuracy and stability.
To use titration standards follow these steps:
1. Select the procedure of interest and order the appropriate
standard. Use the given catalog numbers.
2. Measure the volume of standard to be used as the sample in
the procedure using a TenSette
®
or PourRite™ Ampules whenever
®
Pipet or Class A pipet.
3. Perform the procedure as written, adding deionized water
as necessary.
4. After titrating, the required number of digits should
approximately equal the expected digits.
Call Hach Technical and Customer Service (1-800-227-4224) for
additional help.
19
GENERAL DESCRIPTION, continued
.
Table 1 Titration Standards
Procedure
(Parameter)
Acid-Base:
Standard Description
(Cat. No.)
0.500 N H
(2121-26)1.0
2SO4
Volum e o f
Standard
Acid
Base0.500 N Na
2CO3
(14278-10)
Acidity0.500 N H2SO4 (2121-26)0.1
Alkalinity0.500 N Na
Calcium*:
mg/L CaCO
3
10,000 mg/L CaCO
G.d.h.10,000 mg/L CaCO
(14278-10)0.1
2CO3
(2187-10)
3
3
(2187-10)
Carbon
10,000 mg/L CO
(14275-10)0.2
2
Dioxide
Chloride12,500 mg/L Cl (14250-10)0.1
(mL)
5.0
1.0
5.0
1.0
1.0
0.1
1.0
0.2
1.0
2.0
0.1
1.0
1.0
Titration Cartridge
(Cat. No.)
1.600 N NaOH
(14379-01)
8.00 N NaOH
(14381-01)
1.600 N H2SO4
(14389-01)
8.00 N H2SO4
(14391-01)
0.1600 N NaOH
(14377-01)
1.600 N NaOH
(14379-01)
0.1600 N H2SO4
(14388-01)
1.600 N H2SO4
(14389-01)
0.0800 M EDTA
(14364-01)
0.800 M EDTA
(14399-01)
0.1428 M EDTA
(14960-01)
0.714 M EDTA
(14959-01)
0.3636 N NaOH
(14378-01)
3.636 N NaOH
(14380-01)
0.2256 N Hg(NO
3)2
(14393-01)
0.2256 N AgNO
3
(14396-01)
1.128 N AgNO
3
(14397-01)
2.256 N Hg(NO
)2
3
(921-01)
Expected
Digits
250
250
250
250
250
250
250
250
100
100
112
112
100
125
125
250
125
20
GENERAL DESCRIPTION, continued
Table 1 Titration Standards (Continued)
Procedure
(Parameter)
Standard Description
(Cat. No.)
Chlorine~50 mg/L Cl2
(14268-20)
(see certificate)
~25 mg/L Cl
(26300-20)
Chromate1000 mg/L Cr
(2231 mg/L CrO
(14664-42)
Hardness:
mg/L CaCO
10,000 mg/L CaCO3 (2187-10)
3
G.d.h. 10,000 mg/L CaCO
Iron50 mg/L Fe
(14254-10)
1000 mg/L Fe
(2271-42)
Oxygen,
Dissolved****
Sulfite5000 mg/L SO
10 mg/L as DO
(401-1 1)
3
Volum e o f
Standard
(mL)
2.0
Titration Cartridge
(Cat. No.)
0.02256 N Na
(24091-01)
2
0.5
0.00564 N FEAS
(22923-01)
1.0 0.2068 N Na2S2O3
)
4
0.1
(22676-01)
0.0800 M EDTA
(14364-01)
0.1
0.0800 M CDTA
(14402-01)
1.0
0.800 M EDTA
(14399-01)
1.0
0.800 M CDTA
(14403-01)
(2187-10)0.2
3
0.1428 M EDTA
(14960-01)
1.0
0.714 M EDTA
(14959-01)
10.0
0.0716 M TitraV er
(20817-01)
10.0
0.716 M TitraVer
(20818-01)
100
0.2000 N Na
(22675-01)
200
2.00 N Na
2S2O3
(14401-01)
(22674-10)1.00.3998 N KIO
(14961-01)
2S2O3
2S2O3
–
KI
3
Expected
Digits
varies**
varies***
223
100
100
100
100
112
112
200
100
500
100
250
* One to two drops of Magnesium Standard Solution (10 g/L as CaCO
) must be added to get a sharp
3
end point. These added drops will not change the results.
** The expected digits equal the volume of standard times the concentration on the certificate (e.g., 2 mL
x 50 mg/L = 100 digits).
*** The expected digits equals the volume of standard times the concentration on the certificate times the
constant, 4. (Example: 0.5 mL x 50 mg/L x 4 = 100 digits)
**** Add one Sulfamic Acid Powder Pillow to the volume of standard and follow Steps 10 to 12 in the
Dissolved Oxygen Procedure. It is not necessary to add the first two reagents.
21
GENERAL DESCRIPTION, continued
1.4Adapting a Buret Titration to the Digital Titrator
Adapt any standard titration procedure using a buret to the Digital
Titrator by using the following procedure.
1. Determine the approximate number of digits required. The
Digital Titrator dispenses 1 mL per 800 digits on the counter.
Using the following equation, determine the digits required
for your buret method.
Digits Required
NtmLt800××
-------------------------------------- -=
N
c
Where:
Nt = Normality of buret titrant
mLt = milliliters of buret titrant required for an average titration
= Normality of Digital Titrator cartridge
N
c
2. If the number of digits required is within the range of 70 to
350, you can use the procedure as written, substituting the
Digital Titrator directly for the buret. Or, if the number of
digits is outside of this range, make the
following modifications:
a. If the number of digits required is more than 350, reduce
the sample size to save titrant.
b. If the number of digits required is less than 70, increase
the sample size to increase precision.
c. If the sample size is altered, adjust the amount of
buffering or indicating reagents by the same proportion.
3. When using the Digital Titrator for your buret method, note
the number of digits required for a sample titration. To
convert the digits required to the equivalent number of
milliliters if the buret method was used, calculate:
N
c
Equivalent Buret MillilitersDigits Required
----------------------
×=
800 x N
t
If the sample size was changed, adjust the equivalent buret
milliliters accordingly. If the sample size was increased, reduce
the equivalent buret milliliters; if the sample size was reduced
increase the equivalent buret milliliters. Multiply the equivalent
22
GENERAL DESCRIPTION, continued
buret milliliters by any normally used factors to calculate
concentration in oz/gal, g/L, etc.
Example: Adapt a buret procedure, which normally requires
about 20 mL of a 0.4 N titrant, to the Digital Titrator. Try an 8.0 N
titration cartridge. The first equation above gives:
Digits Required
0.4 20×800×
-------------------------------------80 0 di g its==
Because this would use excessive titrant, reduce the sample size
to one fourth its normal size to reduce the digits required to 200,
well within the recommended range.
Upon completion of the titration using the smaller sample size,
calculate the equivalent buret milliliters by the second equation
above. If 205 were the digits required:
Equivalent Buret Milliliters
Multiply the 5.13 mL by 4 to account for the reduction in sample
size to give the true equivalent buret milliliters of 20.5 mL. If the
buret method called for multiplying the number of milliliters of
titrant by a factor to calculate the concentration of a sample
component, then multiply 20.5 by that factor.
1.5Using PermaChem® Powder Pillows
1. Tap the PermaChem on a hard surface to collect the
powdered reagent in the bottom.
8.0
205 8.0×
------------------------5. 1 3 mL==
800 0.4×
2. Tear across on the dotted pillow line marked “TEAR”
holding the pillow away from your face.
23
GENERAL DESCRIPTION, continued
3. Using two hands, Push both sides toward each other until
thumbs and forefingers form a diamond. Make sure to Crease
the foil pack, so that it forms a spout.
4. Pour the pillow contents into the sample. The polyfilm lining
is specially formulated to deliver all the powder necessary for
accurate results (no tapping on the vessel edge is necessary).
1.6Safety
Safety is the responsibility of each individual when performing
analysis procedures, and the analyst must develop and maintain
good safety habits. Because many of the procedures in this
methods handbook use potentially hazardous chemicals and
apparatus, it is important that the analyst practice good laboratory
techniques to minimize accidents. The following paragraphs
present several techniques applicable to water analysis in the
laboratory and in the field. They are not all inclusive, of course,
nor do they apply only to the procedures provided in this
handbook. They are general in nature but emphasize practices
that are often key factors in personal injury incidents.
•Read labels carefully. Never remove the label from a reagent
container. When preparing a reagent or standard solution, be
sure to label the container clearly and date it.
•A Material Safety Data Sheet (MSDS) comes with each
reagent. This sheet contains helpful information on first aid,
24
GENERAL DESCRIPTION, continued
spill and disposal procedures, and precautionary measures
and should be read before using the product.
•Warning labels also appear on some of the apparatus used
with the test procedures.
•Wear protective clothing when handling chemicals that cause
irritation or burns. Eye protection in particular is important to
guard against spattering and splashes from accidental spills
when caustic materials are being used.
•Use tongs or finger cots when transferring apparatus that
is hot.
•Use mechanical pipetters: Mouth pipetting could result in
accidentally ingesting dangerous chemicals. Make a habit of
using mechanical pipet fillers for all pipetting. This will avoid
mistakes that could cause serious injury.
•Use special care with dangerous chemicals and apparatus.
•Follow the test procedure steps carefully and observe all
precautionary measures. It is good practice to read the entire
procedure carefully before beginning the procedure. Use
safety equipment, such as pipet fillers, protective clothing,
and ventilating hoods, appropriate for the test being
conducted. Wipe up all spills promptly. Do not smoke or eat
in an area where toxic or irritating chemicals are used. Use
reagents and apparatus only as they were meant to be used
and use them only as directed in the test procedure. Do not
use damaged labware and malfunctioning equipment.
25
26
TITRATION PROCEDURES
27
28
ACID-BASE (10 to 4000 mg/L as meq/L)
Acid Determination
Method 8200
1. Select the sample
volume corresponding to
the expected acid
concentration in
milliequivalents (meq)/L
or normality (N) from
Table 1.
Note: See Sampling and
Storage following these
steps.
5. Add the contents of
one Phenolphthalein
Indicator Powder Pillow
and swirl to mix. The
solution should be
colorless.
Note: Four drops of
Phenolphthalein Indicator
Solution may be
substituted for the
Phenolphthalein Indicator
Powder Pillow.
2. Insert a clean
delivery tube into the
appropriate Sodium
Hydroxide Titration
Cartridge. Attach
the cartridge to the
titrator body. See
General Description,
Step-by-Step, for
assembly instructions.
6. Place the delivery
tube tip into the solution
and swirl the flask while
titrating with sodium
hydroxide until a light
pink color forms and
persists for 30 seconds.
Record the number of
digits required.
3. Flush the delivery
tube by turning the
delivery knob to eject a
few drops of titrant.
Reset the counter to zero
and wipe the tip.
Note: For added
convenience use the
®
TitraStir
General Description,
Step 3 in Step-by-Step.
Stir Plate. See
7. Calculate:
Digits Required x
Digits Multiplier =
Milliequivalents per Liter
of Acid
Note: To determine the
normality of the sample,
divide the milliequivalents
per liter obtained by 1000.
4. Use a graduated
cylinder or pipet to
measure the sample
volume from
Table 1 . Transfer the
sample into a clean
250-mL Erlenmeyer
flask. Dilute to about the
100-mL mark with
deionized water, if
necessary.
29
ACID-BASE, continued
Tabl e 1
Range meq/LRange N
Sample
Volume (mL)
Titration
Cartridge
1-4 0.001-0.0041001.6 N NaOH
1.6 N H
4-10 0.004-0.01501.6 N NaOH
1.6 N H
10-40 0.01-0.041008 N NaOH
8 N H
8 N HCl
20-80 0.02-0.08508 N NaOH
8 N H
8 N HCl
50-200 0.05-0.2208 N NaOH
8 N H
8 N HCl
100-4000.1-0.4108 N NaOH
8 N H
8 N HCl
200-800 0.2-0.858 N NaOH
8 N H
8 N HCl
500-20000.5-228 N NaOH
8 N H
8 N HCl
1000-40001-418 N NaOH
8 N H
8 N HCl
2SO4
2SO4
2SO4
2SO4
2SO4
2SO4
2SO4
2SO4
2SO4
Catalog
Number
14379-01
14389-01
14379-01
14389-01
14381-01
14391-01
14390-01
14381-01
14391-01
14390-01
14381-01
14391-01
14390-01
14381-01
14391-01
14390-01
14381-01
14391-01
14390-01
14381-01
14391-01
14390-01
14381-01
14391-01
14390-01
Digit
Multiplier
0.02
0.04
0.1
0.2
0.5
1.0
2.0
5.0
10.0
30
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