Digesdahl® Digestion Apparatus Models 23130-20, - 21-Instrument Manual PDF

23130-18
Digesdahl® Digestion
Apparatus
Models 23130-20, -21
Instrument Manual
© Hach Company, 1989-91, 1995-97, 1999. All rights reserved. Printed in the U.S.A. hm/ct 2/97 8 ed
aa/dk Rev. 2, 9/99
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2
CERTIFICATION
Hach Company certifies this instrument was tested thoroughly, inspected

and found to meet its published specifications when it was shipped from
the factory.
The Digesdahl has been tested and is certified as indicated to the
following instrumentation standards.
Product Safety
Per 73/23/EEC LVD: certified compliant by Hach Company to EN 61010-
1 (IEC1010-1), supporting test records by ETL. Listed by ETL to UL
3101-1 (Listing # H0492805390). Certified by CSA to CSA C22.2 No.
1010.1 (Certification # H0492805390).
Immunity
EN 50082-1 (European Generic Immunity Standard) per 89/336/EEC
EMC: Supporting test records by Hach Company, certified compliance by
Hach Company.
Standards include:
EN 61000-4-2 “1995” (IEC 801-2) Electro-Static Discharge
EN 61000-4-4 “1995” (IEC 801-4) Electrical Fast Transients/Burst
EN 61000-4-5 “1995” (IEC 1000-4-5) Surge
EN 61000-4-11 “1994” (IEC 1000-4-11) Voltage Dips,
Interruptions and Variations
ENV 50140 “1993” (IEC 801-3) Radiated RF Electro-Magnetic Fields
ENV 50141 “1993” Conducted Disturbances Induced by RF Fields
ENV 50204 “1995” Radiated Electro-Magnetic Field from Digital
Telephones.
Emissions
EN 50081-1 (Emissions) per 89/336/EEC EMC: Supporting test records
by TÜV Product Services and Hach Company, certified compliance by
Hach Company.
Standards include:
EN 55014 (CISPR 14) Emissions, Class B Limits
EN 60555-2 Harmonic Disturbances Caused by Electrical Equipment
EN 60555-3 Voltage Fluctuation (Flicker) Disturbances Caused by
Electrical Equipment
iii
CERTIFICATION, continued
Canadian Interference-Causing Equipment Regulation, IECS-003,
Class A:
Supporting test records by TÜV Product Services, certified compliance
by Hach Company.
This Class A digital apparatus meets all requirements of the Canadian
Interference- Causing Equipment Regulations.
Cet appareil numérique de la classe A respecte toutes les exigences du
Règlement sur le matériel brouilleur du Canada.
FCC Part 15, Class "A" Limits: Supporting test records by TÜV Product
Services, certified compliance by Hach Company.
(1) this device complies with Part 15 of the FCC Rules. Operation is
subject to the following two conditions:
(2) this device may not cause harmful interference, and (2) this device
must accept any interference received, including interference that may
cause undesired operation.
Changes or modifications to this unit not expressly approved by the party
responsible for compliance could void the user's authority to operate the
equipment.
This equipment has been tested and found to comply with the limits for a
Class A digital device, pursuant to Part 15 of the FCC Rules. These limits
are designed to provide reasonable protection against harmful
interference when the equipment is operated in a commercial
environment. This equipment generates, uses, and can radiate radio
frequency energy and, if not installed and used in accordance with the
instruction manual, may cause harmful interference to radio
communications. Operation of this equipment in a residential area is
likely to cause harmful interference, in which case the user will be
required to correct the interference at his own expense.
The following techniques of reducing the interference problems are
applied easily:
1. Disconnect power from the Digesdahl to verify that it is the source of
the interference.
2. If the Digesdahl is plugged into the same outlet as the device with
which it is interfering, try another outlet.
3. Move the Digesdahl away from the device receiving the interference.
4. Reposition the receiving antenna for the device receiving
the interference.
5. Try combinations of the above.
iv
TABLE OF CONTENTS
CERTIFICATION .................................................................................................................... iii
SPECIFICATIONS.................................................................................................................. vii
SAFETY PRECAUTIONS .................................................................................................... viii
OPERATION
SECTION 1 GENERAL DESCRIPTION ............................................................................ 3

1.1 Introduction ......................................................................................................................... 3
1.2 Scope of Instructions........................................................................................................... 3
SECTION 2 PREPARATION FOR USE .............................................................................. 5

2.1 Unpacking ........................................................................................................................... 5
2.2 Assembly............................................................................................................................. 6
2.2.1 Heater Assembly........................................................................................................ 6
2.2.2 Fractionating Head System........................................................................................ 7
2.3 Selecting a Temperature Setting.......................................................................................... 9
SECTION 3 SAFETY & ENVIRONMENTAL CONSIDERATIONS............................. 11

3.1 Digesdahl Digestion Apparatus......................................................................................... 11
3.2 Using Hydrogen Peroxide ................................................................................................. 12
3.3 Using Sulfuric Acid........................................................................................................... 14
3.4 Clean Up of Spills and Leaks............................................................................................ 14
3.5 Waste Management ........................................................................................................... 15
CONSIDERATIONS DE SECURITE ET D’ENVIRONNEMENT....................................... 16
3.6 Minéralisateur Digesdahl .................................................................................................. 16
3.7 Utilisation de l’eau oxygénée............................................................................................ 17
3.8 Utilisation de l’acide sulfurique ........................................................................................ 19
3.9 Nettoyage des déversements et fuites................................................................................ 20
SECTION 4 OPERATION ................................................................................................... 21

4.1 Apparatus Preparation ....................................................................................................... 21
4.2 Digestion ........................................................................................................................... 21
4.2.1 Appropriate Sample Size ......................................................................................... 22
4.2.2 Proper Digestion Solution Temperature .................................................................. 22
4.2.3 Sufficient Sulfuric Acid ........................................................................................... 22
4.2.4 Carbonization Period ............................................................................................... 24
4.2.5 Adequate Peroxide Concentration for Sufficient Time............................................ 24
4.2.6 Containment of Sample ........................................................................................... 25
v
TABLE OF CONTENTS, continued
4.2.7 Sampling and Storage.............................................................................................. 25

4.2.8 Accuracy Check ...................................................................................................... 25
DIGESTION PROCEDURES
GENERAL DIGESDAHL DIGESTION ............................................................................. 29
SAMPLE TYPE AND SIZE................................................................................................... 35
DIGESTION PROCEDURE FOR AQUEOUS LIQUIDS................................................. 39
DIGESTION PROCEDURE FOR OILS............................................................................. 53
DIGESTION PROCEDURE FOR SOLIDS ....................................................................... 67
MAINTENANCE
SECTION 5 MAINTENANCE............................................................................................ 81
5.1 Fuse Replacement ............................................................................................................. 81
5.2 Kit Replacement Parts ...................................................................................................... 81
GENERAL INFORMATION
REPLACEMENT PARTS....................................................................................................... 85
HOW TO ORDER .................................................................................................................. 87
REPAIR SERVICE ................................................................................................................. 88
WARRANTY.......................................................................................................................... 89
vi
SPECIFICATIONS
Temperature Range:
Variable from 100 to 480 ° C (212 to 896 ° F)
Temperature Control:
Within ± 15 ° C of set point*
Power Requirements:
115 and 230 Vac models, 50/60 Hz, 250 W** (use only single phase
for 230 V)
Aspirator Capacity:
11.5 L/min (3.0 gal/min) at water flow rate of 6.5 L/min (1.7 gal/min).
Minimum pressure 51.7 kPa (7.5 psi). Drain required.
Dimensions:
14 cm x 16.5 cm x 33.6 cm (5.5” x 6.5” x 13.25”).
Total height: approximately 61 cm (24”) when assembled for use.
Weight:
Net: 3.85 kg (8.5 lbs)
Shipping: 4.8 kg (10.6 lbs)
Operating Conditions:
15-35 ° C (59-95 ° F); 0-85% relative humidity
* The Digesdahl apparatus may be influenced by electric field radiation of 3 volts per meter or greater at
frequencies of 100 ±15 MHz and 180 ±15 MHz. The temperature specification of ±15 ° C was not exceeded by
more than 10 ° C at these radio frequencies.
** Use only single phase power for 230 V models. The over-temperature protection device may not interrupt power
when using poly-phase power.
vii
SAFETY PRECAUTIONS
Notice
Before attempting to unpack, set up or operate this instrument, please read
this entire manual.
Pay particular attention to Section 3! Failure to do so could result in

serious injury to the operator or damage to the equipment.
The digestion procedures in this manual involve the use of strong acid
and oxidizer at high temperatures. To avoid personal injury, observe
all warning messages.
Use of Danger Messages, Cautions and Notes

Danger messages, warnings, cautions and notes used in this manual have
the following significance:
DANGER
Indicates either a potentially or imminently hazardous situation which,
if not avoided, could result in death or serious injury.
CAUTION
Indicates either a potentially or imminently hazardous situation which,
if not avoided, could 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 instrument, references the Instruction

Manual for operational and/or safety information.
3.1 Digesdahl Digestion Apparatus
3.2 Using Hydrogen Peroxide
3.3 Using Sulfuric Acid
3.4 Clean Up of Spills and Leaks
4.2 Digestion
viii
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 nécessaires et se familiariser avec
toutes les procédures de sécurité avant de manipuler tout produit chimique.
1
2
SECTION 1 GENERAL DESCRIPTION
1.1 Introduction
The Hach Digesdahl Digestion Apparatus shown in Figure 1 is designed
to digest a wide variety of sample types for subsequent determination of
total Kjeldahl nitrogen, several minerals, and nutrients. Sample types
include food products, feeds, grains, wastewater sludges, plating baths,
plant tissues, fertilizers, beverages, and oils.
Digestion takes a fraction of the time required for traditional methods.

The digest is used with colorimetric, turbidimetric or titrimetric
procedures for final measurements. Digesdahl test results compare
favorably in accuracy and precision with those obtained by traditional
analytical methods.
DANGER
This product does not have thermal run-away protection when using
polyphase AC main power systems. Use this instrument only with single
phase 230 VAC systems.
DANGER
Ce produit n’a pas de protection contre la surchauffe lorqu’il est utilisé
sur une alimentation électrique en triphasé. Utiliser cet appareil
seulement sur alimentation 230 V monophasé.
1.2 Scope of Instructions

This manual is a guide and reference for safety recommendations,
assembly, general operation, replacement parts, service and warranty
information. Digestion procedures for the Digesdahl Digestion Apparatus
vary according to the type and form of the sample. Digestions for liquids,
oils and solids are found in this manual.
3
Figure 1 Digesdahl Digestion Apparatus
CAPILLARY
FUNNEL
VENT TRAP
CAP
CAPILLARY
FUNNEL
ADAPTOR
VENT TRAP
BODY
COLLUMN
BAFFLE
FRACTIONATING
COLUMN
COLUMN
RECEPTACLE
SAFETY
VERTICAL SHIELD
SUPPORT
FLASK
HEAT WEIGHT
SHIELD
DIGESTION
FLASK
TEMPERATURE
CONTROL
TEMPERATURE
INDICATOR
POWER
SWITCH
MODE
SWITCH
HEATER
ASSEMBLY
4
SECTION 2 PREPARATION FOR USE
2.1 Unpacking
Remove the Digesdahl Digestion Apparatus and accessories from the
shipping container and inspect each item for any damage that may have
occurred during shipping.
Verify that the following items are present:
• Heater Assembly, with power cord, fuse

• Vertical Support, shielded
• Column Receptacle
• Digestion Flasks (2)
• Flask Weight
• Heat Shield
• Aspirator
• Cooling Pad
• Finger Cots (2)
• Goggles, safety
• Instruction Manual
• Fractionating Head System parts:
• Fractionating Column, w/protector
• Capillary Funnel
• Capillary Funnel Adapter
• Vent Trap Body
• Vent Trap Cap
• Column Baffle Tubing, C-Flex, 6.25 feet
If any items are missing or damaged, please contact the Customer Service
Department, Hach Company, Loveland, Colorado (the toll-free number is
800-227-4224). For customers outside the U.S.A., contact the Hach office
or authorized distributor serving you. Please do not return the instrument
without prior authorization from Hach.
5
2.2 Assembly
2.2.1 Heater Assembly
Assemble the heater assembly as shown in Figure 2.
Figure 2
Heater Assembly
6
2.2.2 Fractionating Head System
The fractionating head system is shown in Figure 3 and includes the
fractionating column, column baffle, the capillary funnel, and the exhaust
system components. Assemble as follows:
1. Place the fractionating column in the column receptacle (shown in

Figure 2) and place the column baffle in the top of the column with the
tapered end up.
2. Insert the capillary funnel adapter into the largest opening of the vent
trap body.
Note: The Hach Fume Scrubber Apparatus can be used in place of the aspirator.
Fumes are drawn into a chemical absorber module and absorbed by an activated
carbon filter. This filter is replaced when the absorbing capacity is exhausted. The
Fume Scrubber is designed for running up to six digestions simultaneously. .
3. Place the vent trap cap on the capillary funnel adapter .

4. Place the assembled capillary funnel adapter and vent trap parts on the
fractionating column.
5. Insert the capillary funnel stem into the hole in the vent trap cap.
6. Install the aspirator in a suitable water tap over a sink. Install the hose
barb fitting in the aspirator side port and install the extension tube.
DANGER
The Hach Fume Scrubber Apparatus can only be used with the
Digesdahl Digestion Apparatus for sulfuric acid digestions. Hazardous
conditions could develop if fumes from an alternate acid are vented with
the Fume Scrubber. It is important to clean the Fume Scrubber after
each use to prevent corrosion (see Operation section of Fume
Scrubber manual).
DANGER
L'épurateur de fumées Hach peut seulement être utilisé avec le
minéralisateur Digesdahl pour des minéralisarions à l'acide sulfurique.
Des conditions de risque peuvent être créées par l'aspiration de vapeurs
d'un autre acide dans l'épurateur de fumées. Il est important de
nettoyer l'épurateur de fumées après chaque utilisation pour éviter
la corrosion.
7. A 6.25-foot length of C-flex tubing is supplied with the aspirator. Cut
a segment approximately 16 inches long and connect the top stem of
the column receptacle to the vent trap body. Cut another segment from
the remaining tubing to connect the aspirator to the lower stem of the
column receptacle. This segment should be kept taut with no drape
that can collect condensate. The fractionating head system is now
assembled for use.
7
Figure 3
Fractionating Column and
Exhaust Assembly
8
2.3 Selecting a Temperature Setting
Note: During a The particular temperature applicable for the sample to be digested is
digestion, the given in the appropriate analysis procedure manual. The steps below
temperature explain how to set the heater temperature.
reading will vary
slightly above and
1. Connect the power cord to the line voltage receptacle and set the
below the
selected POWER switch to ON. The TEMPERATURE indicator will light.
temperature. This
2. Set the Mode switch to SET. The TEMPERATURE indicator will
will not affect the
digestion or the display the current temperature set point in degrees Celsius.
accuracy of the
3. If a different temperature is desired, adjust the Temperature ADJ
final analysis.
When idling (no control for the desired temperature in the digital display.
digestion flask in
4. Set the Mode switch to READ and allow time (approximately
place), the
temperature may 10 minutes) for the heater to reach the selected temperature. With the
fluctuate ± 15 ° C Mode switch in the READ position, the temperature display shows the
from the set point. current operating temperature.
9
10
SECTION 3 SAFETY & ENVIRONMENTAL
CONSIDERATIONS
Each person performing laboratory tests is responsible for safety. The
analyst should develop and practice good safety habits to minimize
chances for accidents by practicing good laboratory techniques.
3.1 Digesdahl Digestion Apparatus

For safe Digesdahl operation, observe the following precautions:
• Sample size -- Never digest a sample which contains over 0.5 g of

material which is not water.
• Oils and organic liquids should be considered as solids when

determining sample size.
• Acid type -- Only use acid specified in Hach step-by-step procedures.

• Acid volume -- Never use less than 3 mL.
• Always follow the order of steps indicated.
• If the sample goes to dryness, remove it from the heat immediately and
cool at room temperature. Never add hydrogen peroxide to a dry
sample flask; an explosion could occur. If you are not sure enough
sulfuric acid is present in the digestion flask, STOP. Do not add
hydrogen peroxide. Begin the digestion again with less sample or
more sulfuric acid.
• Be sure to keep the heat shield and the Digesdahl’s safety shield in
place during use.
• Always perform digestion behind a safety shield (Cat. No. 20974-00) or in

a closed fume hood.
• For respiratory protection, use a fume hood or Hach’s Fume Scrubber

Apparatus (Cat. No. 23266).
• Always wear safety glasses or goggles- be sure they have side shields.
• Wear protective gloves for during digestion procedures. Use tongs or
finger cots to transfer hot apparatus.
• Do not add alcohol, acetone or other organic solvents to the digestion

flask before or after digestion.
• During digestion, use the heat setting and digestion time specified in
the instructions. Do not leave the Digesdahl unattended during use.
11
• When digesting a new substance for the first time, begin with a smaller
size and work up to the optimum quantity for digestion. Do not permit
the flask to boil to dryness.
• Use laboratory coats or aprons to protect skin and clothing

from splashes.
• Wear appropriate shoes to protect feet from spills. Open-toed shoes

should not be worn.
• Do not use damaged glassware or apparatus. Discard all damaged

equipment and replace it.
• Allow the Digesdahl to cool naturally (in ambient air). Cold water may
cause hot glassware to shatter.
3.2 Using Hydrogen Peroxide

DANGER
Hydrogen peroxide is an explosion hazard.
Use these additional specific safety precautions when using hydrogen

peroxide in the Digesdahl digestion applications:
• Do not mix hydrogen peroxide with any chemical reagents except as

specified in the Hach instructions.
• Do not add hydrogen peroxide directly to the column on the digestion

flask. Always add hydrogen peroxide in a slow and controlled manner;
use the capillary funnel.
• Hydrogen peroxide should be added to the organic materials in the

flask only when sulfuric acid is present.
• Do not use hydrogen peroxide in concentrations greater than 50%.

Hydrogen peroxide (30% or 50%) is a powerful oxidant and should never
be stored near flammable materials. Like sulfuric acid, it can cause burns
and eye damage. In case of eye or skin contact, flush eyes and/or skin
with water for 15 minutes. Immediately call a physician.
Hydrogen peroxide is highly corrosive and should be cleaned up with

water if spilled on instruments or a counter top. Read and observe all
warnings on the reagent labels and Material Safety Data Sheets.
12
Proper handling and storage procedures involving hydrogen peroxide
should always address two major characteristics of the product:
• It is a strong oxidizing agent. The chemical nature of hydrogen

peroxide makes it an strong irritant to skin, mucous membranes and
particularly to the eyes. It will cause chemical burns at industrial
concentrations and may cause spontaneous combustion upon
immediate or prolonged contact with combustibles
• It can decompose, releasing heat and oxygen. Normally this rate is

very slow for industrial-grade product, but it will accelerate when
contaminated by materials such as dust, metallic ions, or alkali.
Please observe the following precautions for handling and storing of

hydrogen peroxide:
• Do store in a cool place away from direct sunlight (preferably in

a refrigerator).
• Do store in the original containers with closures as supplied and keep

closed when not in use. (Be sure the containers are vented. Hach hydrogen
peroxide bottles are shipped with a special vented cap liner.)
• Do wear gloves and safety glasses when handling the material.

• Do use silicon carbide boiling chips when digesting liquid samples.
• Do wash contaminated skin and body quickly with plenty of water.
Remove contaminated clothing and wash well before using again.
• Do wash eyes with plenty of water if contaminated and get medical

attention quickly.
• Do get medical advice without delay if the material is ingested.

• Do flush all spills with large amounts of water.
• Do not store near heat sources or in contact with combustible or
organic materials.
• Do not inhale vapors or ingest the material.

• Do not allow contact with eyes or skin.
• Do not allow contact with decomposition catalysts (metals, dust,
alkali, etc.).
13
• Do not use unapproved materials (brass, copper, carbon steel, rubber,
etc.) for transfer or storage systems.
Caps on the reagent bottles are made with a special porous liner that
allows venting of gas. The venting cap always must be used on the bottle
of hydrogen peroxide. As a precaution, the reagent bottles are shipped in a
plastic bag. If there is evidence of leakage during shipment, wear gloves
when removing the bottle from the bag and rinse the bottle with water
when removed from the bag. Rinse the bag before disposal.
3.3 Using Sulfuric Acid

Read and observe all warnings on the reagent labels and Material Safety
Data Sheets that accompany the sulfuric acid.
Concentrated sulfuric acid used in the digestion process should be

handled correctly and with caution. Sulfuric acid is a strong acid and
strong oxidizer; it can cause burns if splashed on the skin and permanent
damage if eye contact occurs. This caustic action is much more severe if
the acid is hot. In case of eye or skin contact, flush eyes and/or skin
with water for 15 minutes. Immediately call a physician.
Sulfuric acid mist or vapor has been classified by the International

Agency for Research on Cancer (IARC) as a possible human carcinogen.
Sulfuric acid is a strong oxidizer. It may ignite or explode on contact with

many different chemicals. Follow proper storage regulations.
3.4 Clean Up of Spills and Leaks

Use extreme caution when cleaning spills and leaks throughout the entire
digestion procedure. Your facility may require that only trained
individuals wearing appropriate protective equipment (gloves, goggles,
face shields and chemical resistant clothing) respond to a spill or leak to
ensure the Digesdahl is properly cleaned.
A spill, overflow, or eruption from the Digesdahl apparatus may leave a

residue on the equipment or other surfaces. Cleaning the residue must be
done cautiously. Do not use alternative cleaning methods or cleaning
agents not authorized or endorsed by Hach Company; they may damage
the equipment.
While cleaning a spill or leak, please follow the safety measures below:
1. DO NOT attempt to clean the apparatus if it is hot; this could cause the
glass to shatter. Let the apparatus cool before cleaning it.
14
2. Unplug the Digesdahl before cleaning.
3. Wear gloves and goggles when handling the glassware. Carefully rinse
the glassware several times with water to decontaminate it.
4. Wipe the exterior surfaces of the Digesdahl apparatus (heating mantle,
electrical controls, etc.) and other laboratory surfaces several times
with a damp or wet cloth or paper towel.
5. Do not rinse or spray the apparatus directly; this could damage
the equipment.
6. Discard any paper towels or cloths in an appropriate manner; they may
be contaminated from the sample or chemical residues.
3.5 Waste Management

Hazardous waste disposal regulations were promulgated in accordance
with the Resource Conservation and Recovery Act (RCRA) and are given
in Title 40 Code of Federal Regulations (CFR), parts 260 to 280. Waste
must be managed and disposed of in accordance with federal, state and
local regulations. Refer to Section VIII of the Hach Material Safety Data
Sheet that come with reagents for basic disposal information on Hach
Products. The USEPA maintains a hotline number for questions regarding
RCRA. It is 1-800-424-9346
This manual does not contain all the regulatory requirements. Additional
state and local laws may apply to waste that you generate. It is each
generator’s responsibility to know which regulations apply to them and to
adhere to these regulations. Check with your environmental compliance
staff for specific instructions.
Section 3 summarizes basic requirements for safely handling the

chemicals used in the Digesdahl digestion. It is a guide only and is not
comprehensive for all parties. The information is not intended to provide
any express or implied warranties to readers. This information is not
intended to form any type of obligation upon Hach Company or
its agents.
For further information, please contact the Hach Environmental Safety

and Health Department at (515) 232-2533.
15
CONSIDERATIONS DE SECURITE ET D’ENVIRONNEMENT
Chaque personne effectuant des analyses de laboratoire est responsable de
la sécurité. L’analyste doit développer et appliquer de bonnes habitudes
de sécurité pour minimiser les risques d’accidents en pratiquant de bonnes
techniques de laboratoire.
3.6 Minéralisateur Digesdahl

Pour une utilisation du Digesdahl en toute sécurité, observer les
précautions suivantes :
• Poids d’échantillon : Ne jamais minéraliser un échantillon qui contient

plus de 0,5 g de produit qui ne soit pas de l’eau.
• Les huiles et liquides organiques doivent être considérés comme des

solides pour la détermination du poids d’échantillon.
• Type d’acide : Utiliser seulement l’acide spécifié dans les techniques

détaillées de Hach.
• Volume d’acide : Ne jamais utiliser moins de 3 ml.

• Toujours suivre l’ordre des opérations indiqué.
• Si la fiole va à sec, la retirer immédiatement du système de chauffage
et la laisser refroidir à la température ambiante. Ne jamais ajouter
d’eau oxygénée à une fiole d’échantillon à sec, une explosion
pourrait se produire. Si vous n’êtes pas sûr que la fiole contienne
assez d’acide sulfurique, ARRETEZ. Ne pas ajouter d’eau oxygénée.
Recommencer l’opération avec une quantité d’échantillon plus petite
ou plus d’acide.
• Prendre soin de maintenir en place la cheminée et le manchon de

sécurité du Digesdahl pendant l’utilisation.
• Toujours effectuer les minéralisations derrière un écran de protection

(# 20974-00) ou sous une hotte fermée.
• Pour une protection respiratoire, utiliser une hotte ou l’épurateur de

fumées Hach (réf. n° 23266).
• Toujours porter des lunettes de sécurité avec protections latérales.

• Porter des gants pour la protection pendant les opérations de digestion.
Utiliser des pinces ou des doigtiers de protection pour déplacer les
objets chauds.
16
• NE PAS ajouter d’alcool, d’acétone ou autre solvant organique dans la
fiole de digestion avant ou après minéralisation.
• Pendant la digestion, utiliser le réglage de température et le temps de

digestion spécifié dans les instructions. Ne pas laisser le Digesdahl
sans surveillance pendant l’utilisation.
• Lors de la minéralisation d’une nouvelle substance pour la première

fois, commencer avec une quantité plus petite avant d’utiliser la
quantité optimale pour l’analyse. Ne pas laisser le contenu de la fiole
s’évaporer à sec.
• Porter une blouse ou un tablier de laboratoire pour protéger la peau et

les vêtements des projections.
• Porter des chaussures appropriées pour protéger les pieds des

déversements de produits. Ne pas porter de chaussures à bout ouvert.
• Ne pas utiliser de verrerie ou appareils endommagés. Eliminer et

remplacer tous les équipements endommagés.
• Laisser le Digesdahl refroidir naturellement (dans l’air ambiant). L’eau

froide peut briser le verre chaud.
3.7 Utilisation de l’eau oxygénée
DANGER Utilisez ces précautions de sécurité supplémentaires spécifiques pour

L’eau oxygénée l’utilisation de l’eau oxygénée dans les minéralisations par le Digesdahl :
(peroxyde
d’hydrogène) • NE PAS mélanger l’eau oxygénée avec d’autres réactifs sauf
sous forme indication précisée dans les procédures d’analyse Hach.
concentrée
• NE PAS ajouter d’eau oxygénée directement dans la colonne de
présente un
fractionnement sur la fiole de digestion. Ajouter toujours l’eau
risque
oxygénée avec un débit lent et régulier, utiliser l’entonnoir à
d’explosion.
capillaire Hach.
• L’eau oxygénée doit être ajoutée à la matière organique carbonisée

dans la fiole, seulement en présence d’acide sulfurique.
• NE PAS utiliser d’eau oxygénée à des concentrations supérieures

à 50%.
17
L’eau oxygénée (30% ou 50%) est un oxydant puissant et ne doit jamais
être stocké près de matières inflammables. Comme l’acide sulfurique,
il peut provoquer des brûlures à la peau et aux yeux. En cas de contact
avec les yeux ou la peau, laver les yeux et/ou la peau à l’eau pendant
15 minutes. Retirer les vêtements contaminés. Appeler un médecin.
L’eau oxygénée est extrêmement corrosive et doit être lavée à l’eau si elle
est répandue sur des appareils ou sur la paillasse. Lire et observer tous les
avertissements sur les étiquettes des réactifs et les fiches de données de
sécurité des produits.
Les procédures de manipulations et de stockage concernant l’eau

oxygénée doivent tenir compte de deux caractéristiques importantes
du produit :
• C’est un agent fortement oxydant. La nature chimique de l’eau

oxygénée en fait un produit irritant pour la peau, les muqueuses
et particulièrement les yeux. Il provoque des brûlures graves aux
concentrations auxquelles il est utilisé dans l’industrie et peut
provoquer une combustion spontanée au contact immédiat ou prolongé
des combustibles.
• Il peut se décomposer avec dégagement de chaleur et d’oxygène. La

vitesse de décomposition naturelle du produit de qualité industrielle
courante est très lente, mais elle s’accélère lorsqu’elle est contaminée
par des substances telles que poussière, ions métalliques, ou alcalines.
Prendre les précautions suivantes pour la manipulation et le stockage de

l’eau oxygénée :
• Stocker dans un endroit frais à l’abri de la lumière directe du soleil

(de préférence dans un réfrigérateur).
• Stocker dans les récipients d’origine avec les bouchons fournis et les
maintenir fermés lorsqu’ils ne sont pas utilisés. (S’assurer que les
récipients sont ventilés. Les flacons d’eau oxygénée Hach sont livrés
avec un joint de bouchon perméable spécial).
• Porter des gants et des lunettes de sécurité lors de la manipulation

du produit.
• Utiliser des grains de carbure de silicium pour régulariser l’ébullition

lors de la digestion d’échantillons liquides.
18
• Laver la peau contaminée rapidement à grande eau. Retirer rapidement
les vêtements contaminés et les laver soigneusement avant de les
réutiliser. Les laver régulièrement.
• Laver les yeux à grande eau s’ils sont contaminés et consulter un

médecin immédiatement.
• Consulter immédiatement un médecin si le produit est ingéré.

• Laver toute trace répandue à grande eau.
• NE PAS stocker près des sources de chaleur ou au contact de
combustibles ou de produits organiques.
• NE PAS laisser le produit stocké ou enfermé dans un espace clos.

• NE PAS inhaler les vapeurs ou ingérer le produit.
• NE PAS mettre le produit au contact des yeux et de la peau.
• NE PAS laisser au contact avec des catalyseurs de décomposition
(métaux, poussières, produits alcalins, etc.).
• NE PAS utiliser de matériaux de construction inadaptés (laiton,

cuivre, acier, caoutchouc, etc.) pour les systèmes de stockage
et tuyauteries.
Les bouchons des flacons de réactifs sont prévus avec un joint poreux
spécial qui permet l’échappement de gaz. Le bouchon d’origine doit
toujours être utilisé sur le flacon d’eau oxygénée. A titre de précaution,
les flacons de réactifs sont expédiés dans un sac plastique. S’il existe des
traces de fuites pendant le transport, porter des gants pour retirer le flacon
du sac et rincer le flacon à l’eau après l’avoir sorti du sac. Rincer le sac
avant élimination.
3.8 Utilisation de l’acide sulfurique

Lire et observer tous les avertissements sur les étiquettes des
produits et la fiche de données de sécurité du produit qui accompagne
l’acide sulfurique.
L’acide sulfurique concentré utilisé dans l’opération de minéralisation

doit être manipulé correctement et avec précaution. L’acide sulfurique
est un acide fort et un oxydant puissant qui peut provoquer des brûlures
graves au contact de la peau et des lésions irréversibles s’il est mis au
contact des yeux. Cette action corrosive est beaucoup plus grave si l’acide
est chaud. En cas de contact avec les yeux ou la peau, laver les yeux et/
19
ou la peau à l’eau pendant 15 minutes. Retirer les vêtements
contaminés. Appeler un médecin.
L’acide sulfurique sous forme de brouillard ou de vapeur a été classé

comme cancérigène possible pour l’homme par l’Agence Internationale
de Recherche sur le Cancer (IARC).
L’acide sulfurique est un oxydant puissant. Il peut provoquer un feu ou

exploser au contact de nombreux produits chimiques différents. Suivre les
règles de stockage appropriées.
3.9 Nettoyage des déversements et fuites

Prendre les plus grandes précautions pour nettoyer des fuites ou produits
répandus pendant toute la technique de digestion. Votre société peut
exiger que seules des personnes habilitées portant les équipements de
protection appropriés (gants, lunettes de sécurité, masques de protection
et vêtements résistants aux agents chimiques) interviennent en cas de
déversement ou de fuite.
Un déversement, débordement ou une projection par le minéralisateur

Digesdahl peut laisser un résidu sur le matériel ou d’autres surfaces. Le
nettoyage du résidu doit être fait avec précaution. Veuillez observer les
mesures de sécurité ci-dessous :
1. NE PAS tenter de nettoyer l’appareil pendant qu’il est chaud, ceci

peut causer la rupture du verre. Laisser refroidir l’appareil avant de
le nettoyer.
2. Débrancher le Digesdahl avant de le nettoyer.
3. Porter des gants et des lunettes de protection pour la manipulation de

la verrerie. Rincer soigneusement la verrerie plusieurs fois à l’eau pour
la décontaminer.
4. Essuyer les surfaces extérieures de l’appareil Digesdahl

(plaque chauffante, commandes électriques, etc.) et autres
surfaces du laboratoire plusieurs fois avec un tissu humide ou
un papier d’essuyage.
5. Ne pas rincer ou arroser l’appareil directement, ceci pourrait

le détériorer.
6. Eliminer les papiers et tissus de façon appropriée, ils peuvent avoir été
contaminés par l’échantillon ou les résidus chimiques.
20
SECTION 4 OPERATION
4.1 Apparatus Preparation
See SECTION 3 for more safety information. Prepare to perform the
digestion either behind a laboratory safety shield or inside a fume hood. If
a fume hood is used, check the fume exhaust system to verify it is
working property.
Safety glasses and protective clothing are mandatory.
Turn on the water to the aspirator to maximum flow. Remove the
capillary funnel and place a finger over the opening in the vent trap cap. A
distinct suction should be felt.
4.2 Digestion
Procedures for using the Digesdahl Digestion Apparatus vary with sample
type. Most procedures use a two-phase digestion process involving
concentrated sulfuric acid and 50% hydrogen peroxide. Sulfuric acid
dehydrates and chars the sample. Hydrogen peroxide is added via the
capillary flow funnel to complete sample decomposition. The capillary
funnel feeds hydrogen peroxide into the digestion flask at a rate of 3 mL
per minute. This allows the analyst to control the amount of time sample
is exposed to the hydrogen peroxide (digestion time) by varying the
volume of hydrogen peroxide used.
DANGER
Wear protective eye glasses and clothing. A strong acid (concentrated sulfuric acid) and
a strong oxidant (50% hydrogen peroxide) are used in the digestion reaction. These
chemicals can cause burns if splashed on the skin or permanent eye damage if allowed
to contact the eyes. If the chemicals are hot, effects are considerably more severe.
Immediately rinse any affected area thoroughly with water and contact a physician.
DANGER
Porter des lunettes et vêtements de protection. Un acide fort (acide sulfurique concentré)
et un oxydant puissant (peroxyde d'hydrogène à 50%) sont utilisés dans la réaction de
minéralisation. Ces produits chimiques peuvent causer des brûlures s'ils sont projetés sur
la peau ou des blessures irréversibles aux yeux s'ils sont mis au contact des yeux. Si ces
produits sont chauds, les effets sont considérablement plus graves. Immédiatement rincer
toute partie atteinte abondamment à l'eau et consulter un médecin.
Use the Digesdahl Digestion Apparatus only behind a laboratory safety

shield or in a closed fume hood.
Some samples are more difficult to digest completely. In a careful study
of the minimal time required to digest a variety of materials, complete
nitrogen recovery was achieved for many samples immediately upon
clearing of the digest (when the digest becomes colorless). However,
resistant or refractory materials such as nicotinic acid require several
minutes of continued peroxide digestion after clearing to obtain 100%
nitrogen recovery.
21
A general procedure, incorporating application specific requirements, is
provided in this section of the manual. To ensure complete sample
digestion, consider the variables described in the following paragraphs.
4.2.1 Appropriate Sample Size

For solid or organic liquid samples, less than 0.5 grams of anhydrous
material can usually be digested effectively. (As a routine practice, 0.25 g
of sample is used.) Samples that contain water may be scaled up by a
proportional amount. There is no restriction or minimum sample size. For
samples of aqueous solutions or suspensions, the maximum volume is 40
mL. When the percent solids exceeds 1% of the sample volume, the
maximum sample volume should be reduced using the formula:
40
sample = --------------------
% solids
4.2.2 Proper Digestion Solution Temperature

Digestion temperature is critical. If the hydrogen peroxide is added to a
cold digestion mixture followed by heating, the hydrogen peroxide
decomposes before the digest reaches the proper temperature. Addition of
hydrogen peroxide to a digest that is too hot volatilizes most of the
oxidant with little benefit. Also, excessive heat contributes to spray loss
of sample as a fine mist. The temperature recommended for most samples
is 440 ° C (825 ° F). For oils, fuels and lubricants, the temperature may
need to be decreased.
4.2.3 Sufficient Sulfuric Acid

The amount of concentrated (specific gravity 1.84) sulfuric acid used
must be sufficient to prevent the digestion from going to dryness. Any
portion of the flask bottom that becomes dry will overheat and may cause
the flask to explode. Also, too little acid will cause the sample to
overheat, which may cause thermal decomposition of desired analytes
(i.e., ammonium compounds) and result in sample loss. Use an amount of
sulfuric acid that will leave at least 2 mL of residual acid when digestion
is complete. Refer to Table 1 for recommended volumes.
22
Table 1 Digestion Guidelines of Specific Sample Types
Preheat
Sample Vol. of Vol. of
Sample Weight Time Special Instructions
Type Acid Peroxide
(Step 5)
Plant tissue 0.25 to 0.5 g 4 mL 4 min. 10 mL Use Nitrogen-free paper to
weigh samples.
Meat & 0.5 g or 4 mL or as in 4 min. 10 mL —
Poultry predigestion predigest
Fluid 0.1 to 0.25 g 4 mL 4 min. 10 mL Add 0.4 g Kjeldahl Reduction
Fertilizers Powder to flask before adding
sulfuric acid. Place the flask in
an 80 °C oven 15 minutes before
digestion. Use N-free paper to
weigh samples.
Feed & 0.25 g 4 mL 4 min. 10 mL —
Forage
Dairy 0.25 to 2.0 g 4 mL 4 min. 10 mL —
Cereal 0.25 to 0.5 g 4 mL 4 min. 10 mL Use Nitrogen-free paper to
weigh samples.
Beverage about 5 g 4 mL 1 min. 10 mL Preheat acid for 1 minute then
(pipet into funnel add sample through funnel. Heat
flask for 30 seconds after sample
is in the flask.
Sludge <2.5 g wet sludge 4 mL 3-5 min. 10 mL of Heat the diluted digest for 15
<0.5 g dried sludge increase in 5 minutes and filter.
mL increments
Water & not more than 0.5 g 3 mL until acid 10 mL or Water must evaporate before
Wastewater solid (mL = 40/C; is refluxing increase in 5 acid will reflux. Boiling chips
C= % solids) mL increments required.
Bath 0.3 to 10 mL 4 mL 4 min. 10 mL Water must evaporate before
Solutions acid will reflux. Boiling chips
required.
Edible Oils 0.25 to 0.5 g 4-6 mL 4 min. 5 mL Weigh samples into flake and
immediately record exact weight.
and 5 mL later
Ion equivalent of 0.25 g 10-15 mL 12 min. 20 mL Digest will be clear with particles
Exchange dry resin on bottom if metal oxides are not
Resins soluble in H2SO4. Add aqua
reagia or suitable solvent to
dissolve particles. If particles are
floating, start again using 15 mL
H2SO4 and longer char time.
Soil 0.25 to 0.5 g 6 mL 4 min. 10-20 mL —

Fuels 0.25 to 0.5 g 6 mL 4 min. 20 mL Heat the diluted digest for 15
min. and filter. Lower heater
temperature if foaming or
burning occurs.
23
Sulfuric acid (H2SO4) consumption depends on the anhydrous mass of
material and the chemical composition of the substance. Use of 4 mL
H2SO4 is suitable for many materials, but not all. Therefore, the analyst
must pay attention to the amount of residual H2SO4 for the type of sample
digested, and adjust the amount of acid or sample accordingly. Never use
less than 3 mL of concentrated sulfuric acid. Larger volumes of H2SO4
may be used, but avoid a large excess since sample pH adjustment is
required in most subsequent determinations.
4.2.4 Carbonization Period
A carbonization period prior to the addition of hydrogen peroxide
provides a reducing environment which helps convert organic nitrogen to
ammonia. In the presence of oxidizable carbon compounds, sulfuric acid
reacts to produce sulfur dioxide, which is the active reducing agent.
The reaction is:
H2SO4 → H2O + SO2 + ½ O2
A preheat period of 2 to 5 minutes is recommended for routine digestions.

4.2.5 Adequate Peroxide Concentration for Sufficient Time
Researchers believe that hydrogen peroxide (H2O2) reacts immediately
with H2SO4 at digestion temperature to give H2SO5 (peroxymonosulfuric
acid) by the reaction:
H2SO4 + H2O2 → H2SO5 + H2O
This is an extremely powerful oxidizing agent toward carbonaceous

material. The objective is to maintain an adequate concentration of H2SO5
in the hot digestion mixture for a long enough time to complete oxidation
of the carbonaceous material. The H2O2 is metered into the flask at
3 mL/min. using the capillary funnel.
The amount of peroxide that must be added for complete digestion can be
determined by digesting a sample multiple times with incremental
increases in the amount of peroxide added (i.e., 5 mL, 10 mL, 15 mL, 20
mL). Results of the analysis for the parameter of interest may then be
graphed to determine the minimum amount of peroxide needed for
optimum sample digestion.
The preferred and recommended peroxide reagent is 50% hydrogen
peroxide. Research studies have shown that the best recovery and
reproducibility are achieved using the 50% peroxide reagent. The 50%
hydrogen peroxide reagent produces dependable results in research and
actual applications. The optimal rate of peroxide addition has been
determined as 3 mL/minute using the 50% reagent. This may not hold
true if other strengths of hydrogen peroxide are used.
24
If 50% hydrogen peroxide is not available, 30% peroxide may be used as
a last resort with caution. Because of the lesser strength, at least
1.67 times more volume must be used (i.e., 16.7 mL of 30% vs. 10 mL of
50% peroxide). Always run a digestion standard, either glycine
p-toluenesulfonate or nicotinic acid p-toluenesulfonate, when using
30 percent peroxide to check completion of the digestion. All
recommended safety precautions apply to both strengths of the hydrogen
peroxide. See Section 3, Safety Considerations.
4.2.6 Containment of Sample

Loss of sample from the digestion flask can occur in two ways:
(1) foaming or boiling over, and
(2) mist or spray in the ventilation air stream.
Foaming is a serious problem with certain sample types, so special
techniques have been developed. Some liquid samples, especially those
containing sugars, cannot be digested by the standard procedure, which
consists of placing a given volume in the flask, adding sulfuric acid and
heating. Under those conditions, foaming cannot be controlled. Instead,
the sulfuric acid is heated in the flask and the liquid sample is added
through the capillary funnel. Carbonization proceeds in a controlled
manner. When all the sample has been added, the peroxide treatment
begins and the digestion continues normally. Other ways to control
foaming include early addition of hydrogen peroxide and reducing the
temperature during carbonization.
Sample loss as spray or mist occurs when small droplets of liquid are
swept out of the flask along with gases, and escape in the ventilation air
stream. The current fractionating column design reduces spray loss to an
insignificant level.
4.2.7 Sampling and Storage

Samples must be homogeneous to ensure that a representative portion is
analyzed. Liquid samples should be homogenized via stirring or blending.
Solid samples should be finely ground or chopped and well mixed. After
digestion, samples should be diluted to the mark, mixed, and tightly
sealed. The diluted digestate will be stable for 2 to 3 days, as long as
evaporation does not occur.
4.2.8 Accuracy Check

Complete digestion is necessary for accurate results. The Digesdahl
system may be checked with Primary Standards for Kjeldahl Nitrogen
using one of the following methods.
25
Solid Samples
1. Weigh 0.25 grams of a Primary Standard for Kjeldahl Nitrogen.
Digest the standard following the general digestion procedure.
2. Any of the three standards may be used. Ammonium p-toluenesulfonate
(185.5 mg/L TKN) is the least difficult to digest. Glycine
p-toluenesulfonate (141.63 mg/L TKN) is moderately difficult to digest,
and Nicotinic Acid p-toluenesulfonate (118.58 mg/L TKN) is the most
difficult to digest.
Liquid Samples
1. Weigh 10.000 grams of a Primary Standard for Kjeldahl Nitrogen.
2. Transfer to a 1-liter volumetric flask and dilute to the mark.
3. Using a volumetric pipet, add 15 mL of the prepared solution to the
digestion flask and digest the standard following the general
digestion procedure.
4. Any of the three standards may be used. Ammonium
p-toluenesulfonate (111.03 mg/L TKN) is the least difficult to digest.
Glycine p-toluenesulfonate (84.98 mg/L TKN) is moderately difficult
to digest, and Nicotinic Acid p-toluenesulfonate (71.15 mg/L TKN) is
the most difficult to digest.
A primary standard set, containing one bottle of each of the standards,
may be purchased from Hach Company. Table 2 lists some of the
properties of the three primary standards.
Table 2 Some Properties of Kjeldahl Nitrogen Standards (#22778-00)
Ammonia PTSA Glycine PTSA Nicotinic Acid PTSA
Formula C7H11O3SN C9H13O5SN C13H13O5SN
Structure
Molecular Weight 189.235 247.277 295.316

Melting Point, °C — 199 179
% Nitrogen 7.402 5.664 4.743
% Protein 46.261 35.403 29.643
Digestability Index 0 3 10
Moisture
Absorption
at 25 % RH 0.04% 0.03% 0.00%
at 50% RH 0.07% 0.047% 0.01%
at 90% RH 0.14% 0.15% 0.08%
26
DIGESTION PROCEDURES
27
Danger
Review Section 3 for important safety information before
performing this digestion procedure.
Danger
Lire au chapitre 3 les informations importantes pour la
sécurité avant d’effectuer cette technique de digestion.
28
GENERAL DIGESDAHL DIGESTION
1. Transfer a 2. Add concentrated 3. Turn on the water to 4. Place the flask

preweighed or a sulfuric acid (according the aspirator and make weight followed by the
premeasured amount of to Table 1 on page 22) to sure there is suction to fractionating column
sample into a 100-mL the volumetric flask and the fractionating with funnel on the flask.
Digesdahl digestion at least two silicon column. Turn the Place the flask on the
flask; see Table 1 on carbide boiling chips for temperature dial to a heater and heat until the
page 22. The amount liquid samples. heat setting of 440 ° C sulfuric acid boils
transferred should not Note: Pretreat boiling (825 ° F). For meat (refluxing sulfuric acid
contain more than 0.5 g chips by soaking in 1:1 digestion, set to 468 ° C will be visible).
of solids or organic Nitric Acid and rinsing (875 ° F). Note: White acid vapors
liquids. The maximum thoroughly with deionized Note: Wait for the proper usually will be present, but
volume for water water. Treatment is very temperature to be reached their presence alone does
samples is 40 mL. In important in low-level before the sample is placed not indicate that the boiling
samples with more than work. Hach recommends on the heater. point of sulfuric acid has
silicon carbide boiling been reached.
1% solids present, use
chips.
the formula below: Note: Liquid samples
require total evaporation of
Water Sample Volume water before vapors
= 40 ÷ % solids are visible.
Note: Use only Hach Note: If sample foams up
digestion flasks. Volumetric into the neck of the flask,
flasks with concave bottoms lower temperature to
should not be used. 335 ° C (635 ° F). Continue
Note: If solids are 10% of heating at lower
total volume of sample, the temperature until all water
maximum volume of liquid is evaporated. Then return
sample would be 4 mL. to original digestion
temperature.
Note: Several 40-mL
sample aliquots of the Note: If foaming or
sample may be digested in bumping is not stopped by
succession to concentrate lowering temperature or
a sample. volume, then liquid samples
that will not clog the
Note: If liquid is too
capillary funnel may be
viscous to measure,
added to the flask via the
preweigh the sample into
capillary funnel, 10 mL at a
the digestion flask.
time. Decrease amount
added if foaming persists.
29
GENERAL DIGESDAHL DIGESTION, continued
3-5 minutes
5. Heat 3-5 minutes. 6. Do not proceed if 7. After addition of 8. Take the hot flask off
Do not boil sample sulfuric acid is not hydrogen peroxide is the heater and allow the
to dryness. If sulfuric visible in the flask. Add complete, boil off excess flask to cool. Remove
acid is not present after 10 mL of 50% Hydrogen hydrogen peroxide by the fractionating column
heating, do not proceed Peroxide to the charred heating for one more from the digestion flask.
with Step 6. Discard the sample via the funnel on minute. Do not heat Note: Use finger cots to
sample if it evaporates to the fractionating head. to dryness. remove the digestion flask.
dryness. Start over and Note: Visually confirm the Note: If the sample goes Place it on a cooling pad
use a larger volume of presence of sulfuric acid in to dryness, turn off the for at least one minute.
sulfuric acid in Step 2 of the flask before adding Digesdahl and air cool to Then remove the column.
this procedure. Or chose hydrogen peroxide. room temperature. Add
a smaller sample amount Note: If the digest does not water to flask before
for digestion. turn colorless, add handling. Repeat the
5 mL increments of digestion from the Step 1
Note: Some organic
peroxide until the digest using a new sample.
samples may need more
than five minutes for becomes clear.
complete digestion. See Note: Use long-neck
Table 1 on page 22. glassware or a pipet
to transfer the
hydrogen peroxide.
30
Use metals or
TKN procedure
9. Dilute the digest with 10. Turn the 11. If the sample has 12. Continue the
approximately 70 mL of temperature dial to a visible turbidity, filter analysis using one of the
deionized water. If not heat setting of 204 ° C or wait until the following procedures.
analyzing for aluminum, (400 ° F). Add 150 mL of turbidity settles, and the
nickel or iron, dilute to water to a 400-mL upper portion of the
the beaker. Place the beaker sample is clear.
100-mL mark with on the heater. Place the Filter as follows:
deionized water; skip flask in the beaker and
Step 10 and proceed to boil for 15 minutes. a) Place a filter paper into
the filter holder with
Step 11. If analyzing for Air cool to room
wrinkled surface upward.
nickel, aluminum or temperature and dilute to
iron, go to Step 10. the 100-mL mark with b) Place the filter holder
deionized water. Invert assembly in the filtering
Note: Add deionized
flask and wet the filter with
water slowly at first. Cool several times to mix.
deionized water to ensure
the flask if necessary
adhesion to the holder.
for handling.
c) While applying a
vacuum to the filtering
flask, transfer the sample to
the filtering apparatus.
d) Slowly release the
vacuum from the filtering
flask and transfer to
another container.
31
Metals Procedure
Note: If analyzing aliquots smaller than 0.5 mL, pH adjustment is unnecessary.
1. Pipet the appropriate analysis volume into the appropriate mixing

graduate cylinder. See Sample and Analysis Volume Tables following
the specific digestion for liquids, solids or oils to determine the
analysis volume.
Note: Some methods require pipetting into a volumetric flask or a regular
graduate cylinder.
2. Dilute to about 20 mL with deionized water.

3. Add one drop of 2,4 Dinitrophenol Indicator Solution.
4. Add one drop of 8 N Potassium Hydroxide (KOH) Standard Solution,
swirling between each addition, until the first flash of yellow appears
(pH 3). If analyzing for potassium, use 5 N sodium hydroxide instead.
Do not use a pH meter if analyzing for potassium or silver.
5. Add one drop of 1 N KOH. Stopper the cylinder and invert several
times to mix. If analyzing for potassium, use 1 N sodium hydroxide
instead.
Note: Use pH paper to insure the pH is 3. If it is higher than 4, do not readjust
with acid; start over with a fresh aliquot.
6. Continue to add 1 N KOH in this manner until the first permanent

yellow color appears (pH 3.5-4.0).
Note: High iron content will cause precipitation (brown cloud) which will co-
precipitate other metals. Repeat this procedure with a smaller aliquot volume.
7. Add deionized water to the volume indicated in the colorimetric

procedure for the parameter you are analyzing. Fill a second graduated
mixing cylinder to the same volume with deionized water.
8. Continue with the colorimetric procedure for the parameter you
are analyzing.
32
TKN, Colorimetric Methods
Consult the spectrophotometer or colorimeter procedure to complete the
TKN analysis. The following is only a guide to use if a procedure is
not available.
1. Pipet an appropriate analysis volume into a graduated mixing cylinder.

2. Add one drop of TKN Indicator.
3. Add one drop of 8 N KOH Standard Solution, swirling between each
addition, until the first flash of pale blue appears (pH 3).
times to mix.
Note: View the cylinder from the top against a white background. Compare the
cylinder against a second cylinder filled to the same volume with deionized water.
5. Continue to add 1 N KOH in this manner until the first permanent blue
color appears.
procedure.
7. Continue with the colorimetric procedure.
33
34
SAMPLE TYPE AND SIZE
Although the Digesdahl can digest many types of samples, a specific
digestion is required for specific sample types. To classify the sample as a
liquid, oil or solid, use the following charts. Follow the appropriate
procedure indicated for each sample type.
Sample size varies, depending on the sample type and the parameter being
measured. Once the correct sample type is decided, use the tables
following each of the digestion procedures to determine the sample size.
Chart 1
For Aqueous Liquids
35
SAMPLE TYPE AND SIZE, continued
Chart 2
For Oils
36
SAMPLE TYPE AND SIZE, continued
Chart 3
For Solids*
*High levels of iron may interfere with analysis of some parameters.
37
Danger
Danger
38
DIGESTION PROCEDURE FOR AQUEOUS LIQUIDS
1. Transfer a 2. Add 3 mL of 3. Turn the temperature 4. Place the flask

premeasured amount of concentrated sulfuric dial to a heat setting of weight followed by the
sample into a 100-mL acid (spec. gravity 1.84) 440 ° C (825 ° F). When fractionating column
Digesdahl digestion to the volumetric flask the proper temperature is with funnel on the flask.
flask; see Sample and and two or more silicon reached, turn on the Place the flask on the
Analysis Volume Tables carbide (carborundum) water to the aspirator heater and heat until the
for Aqueous Liquids boiling chips for liquid and make sure there is sulfuric acid boils
following this samples. suction to the (refluxing sulfuric acid
procedure. The amount Note: Pretreat boiling fractionating column. will be visible).
transferred should not chips by soaking in 1:1 Note: Wait for the proper Note: White acid vapors
contain more than 0.5 g Nitric Acid and rinsing temperature to be reached will usually be present but
of material which is not thoroughly with deionized before sample is placed on their presence alone does
water. The maximum water. Treatment is very the heater. not indicate that the boiling
volume for water important in low-level Note: Always operate the point of sulfuric acid has
samples is 40 mL. In work. Hach recommends Digesdahl apparatus with been reached.
using silicon carbide a safety shield in place or Note: Aqueous samples
samples with more than
boiling chips. inside a closed fume require total evaporation
1% solids present, use
the formula below: hood. Safety glasses of water before vapors
are mandatory. are visible.
Water Sample Volume
= 40 ÷ %solids
Note: If sample foams up
into the neck of the flask,
Note: Use only Hach lower temperature to
Digesdahl flasks. 335 ° C (635 ° F). Continue
Volumetric flasks with heating at a lower
concave bottoms should not temperature until all water
be used. is evaporated. Then return
Note: If solids are 10% of to original digestion
total volume of sample, the temperature.
maximum volume of liquid Note: If foaming or
sample would be 4 mL. bumping is not stopped by
Note: Oils and organics lowering temperature or
should be considered as volume, then liquid samples
solids when determining that will not clog the
sample size. capillary funnel may be
Note: If liquid is too added to the flask via the
viscous to measure, capillary funnel, 10 mL at a
preweigh the sample into time. Decrease amount
the digestion flask. added if foaming persists.
39
DIGESTION PROCEDURE FOR AQUEOUS LIQUIDS, continued
4:00
5. Boil 4 more minutes. 6. Do not proceed if 7. After addition of 8. Take the hot flask off
Do not boil the sample sulfuric acid is not hydrogen peroxide is the heater and allow the
to dryness. If sulfuric visible in the flask! Add complete, boil off excess flask to cool. Remove
acid is not present in the 10 mL of 50% Hydrogen hydrogen peroxide by the fractionating column
flask after the 4 minute Peroxide to the charred heating for one more from the digestion flask.
heating, do not proceed sample via the funnel on minute. Do not heat Note: Use finger cots to
with Step 6! Discard the fractionating column. to dryness. remove the digestion flask.
sample if it evaporates to Note: Visually confirm the Note: If the sample goes Place it on a cooling pad
dryness. Start over and presence of sulfuric acid in to dryness, turn off the for at least one minute.
use a larger volume of the flask before adding Digesdahl and air cool to Then remove the column.
sulfuric acid in Step 2 of hydrogen peroxide. room temperature. Add Do not add water to the
flask until it has cooled.
this procedure. Or Note: If the digest does not water to flask before
choose a smaller sample turn colorless, add 5 mL handling. Repeat the
amount for digestion. increments of hydrogen digestion from the
peroxide until the digest beginning using a new
becomes clear or does not sample.
change color.
Note: If sample foams
during peroxide addition,
remove the Digesdahl
digestion flask and
fractionating column (use
finger cots). Starting with
Step 1, repeat the digestion
adding only 2 mL of
hydrogen peroxide. Then
follow with 8 mL of
hydrogen peroxide.
Note: Do not heat
to dryness.
40
9. Dilute the digest to 10. If analyzing for 11. Turn the 12. If the sample has
approximately 70 mL aluminum, nickel or temperature dial to a visible turbidity, filter or
with deionized water. iron, continue to Step 11. heat setting of 204 ° C wait until the turbidity
Note: Add deionized water If analyzing for other (400 ° F). Add 150 mL of settles, and the upper
slowly at first. Cool the substances, dilute to the water to a 400-mL portion of the sample
flask if necessary 100-mL mark with beaker. Place the beaker is clear.
for handling. deionized water; skip on the heater. Place the Filter as follows:
Step 11 and go to flask in the beaker and
Step 12. boil for 15 minutes. Air a) Place a filter paper into
cool to room
temperature and dilute to
the 100-mL mark with b) Place the filter holder
deionized water. Invert assembly in the filtering
flask and wet the filter with
several times to mix.
deionized water to ensure
adhesion to the holder.
c) While applying a
vacuum to the filtering
another container.
Continue with the
analysis using the
appropriate procedure
below.
Metals Method
Note: If analyzing aliquots smaller than 0.5 mL, pH adjustment is not necessary.
graduate cylinder. See Sample and Analysis Volume Tables for
Aqueous Liquids following this procedure to determine the
analysis volume.
graduate cylinder.
41
instead.
Note: Use pH paper to insure the pH is 3. If it is higher than 4, do not readjust with
acid; start over with a fresh aliquot.
Note: High iron content will cause precipitation (brown cloud) which will co-
precipitate other metals. Repeat this procedure with a smaller aliquot volume.
are analyzing.

not available.

3. Add 8 N KOH Standard Solution, one drop at a time, swirling between
each addition, until the first flash of pale blue appears (pH 3).
times to mix.
color appears.
42
6. Add deionized water to the volume indicated in the
colorimetric procedure.
Sample and Analysis Volume Tables for Aqueous Liquids

The values in these tables reflect the Hach Spectrophotometer with the
narrowest concentration range.
Aluminum, Aluminon (Method 8012)
Expected Al Sample Analysis

Dilute to
conc. (mg/L) amount (mL) Volume (mL)
0.1-5 40.0 20.0 50.0 mL
0.5-20 20.0 10.0 50.0 mL
2.0-80 10.0 5.00 50.0 mL
20-800 5.00 1.00 50.0 mL
200-8000 1.00 0.50 50.0 mL
A × 5000
------------------------ = mg/L Total Al
B× C
A = mg/L reading from instrument
B = mL sample amount from table
C = mL analysis volume from table
Aluminum, ECR (Method 8326)

Dilute to
0.05-1.3 40.0 20.0 50.0 mL
0.2-5.5 20.0 10.0 50.0 mL
0.8-22 10.0 5.00 50.0 mL
8.0-220 5.00 1.00 50.0 mL
80-2200 1.00 0.50 50.0 mL
A × 5000
------------------------ = mg/L Total Al
B× C
43
Cadmium, Dithizone (Method 8017)
Expected Cd Sample Analysis

Dilute to
conc. (µg/L) amount (mL) Volume (mL)
0.05-2.5 40.0 20.0 250 mL
0.2-10 20.0 10.0 250 mL
1-40 10.0 5.00 250 mL
10-400 5.00 1.00 250 mL
100-4000 1.00 0.50 250 mL
A × 25 = µg/L Total Cd
-----------------
B× C
A = µg/L reading from instrument
Chromium, Total (Method 8024)
Expected Cr Sample Analysis

Dilute to
0.05-1.8 40.0 20.0 25.0 mL
0.20-7.5 20.0 10.0 25.0 mL
0.75-30 10.0 5.00 25.0 mL
7.5-300 5.00 1.00 25.0 mL
75-3000 1.00 0.50 25.0 mL
A × 2500
------------------------ = mg/L Total Cr
B× C
44
Cobalt (Method 8078)
Expected Co Sample Analysis

Dilute to
0.1-6.0 40.0 20.0 25.0 mL
0.5-25 20.0 10.0 25.0 mL
2.0-100 10.0 5.00 25.0 mL
20-1000 5.00 1.00 25.0 mL
200-10000 1.00 0.50 25.0 mL
A × 2500- = mg/L Total Co

-----------------------
B× C
Copper, Bicinchoninate (Methods 8026 and 8506)
Expected Cu Sample Analysis

Dilute to
0.25-15 40.0 20.0 25.0 mL
1-60 20.0 10.0 25.0 mL
4-240 10.0 5.00 25.0 mL
40-2400 5.00 1.00 25.0 mL
400-24000 1.00 0.50 25.0 mL
A × 2500
------------------------ = mg/L Total Cu
B× C
45
Iron, 1,10 Phenanthroline (Method 8008)
Expected Fe Sample Analysis

Dilute to
0.15-8 40.0 20.0 25.0 mL
0.6-35 20.0 10.0 25.0 mL
2.5-125 10.0 5.00 25.0 mL
25-1250 5.00 1.00 25.0 mL
250-12500 1.00 0.50 25.0 mL
A × 2500- = mg/L Total Fe

-----------------------
B× C
Iron, Ferrozine (Method 8147)

Dilute to
0.07-4 40.0 20.0 25.0 mL
0.3-15 20.0 10.0 25.0 mL
1.1-65 10.0 5.00 25.0 mL
11-650 5.00 1.00 25.0 mL
110-6500 1.00 0.50 25.0 mL
A × 2500
------------------------ = mg/L Total Fe
B× C
46
Lead, Dithizone (Method 8033)
Expected Pb Sample Analysis

Dilute to
conc. (µg/L) amount (mL) Volume (mL)
0.1-5.0 40.0 20.0 250 mL
0.4-20 20.0 10.0 250 mL
1.5-80 10.0 5.00 250 mL
15-800 5.00 1.00 250 mL
150-8000 1.00 0.50 250 mL
A × 25 = µg/L Total Pb
-----------------
B× C
A = µg/L reading from instrument
Manganese, PAN (Method 8149)
Expected Mn Sample Analysis

Dilute to
0.05-2.1 40.0 20.0 25.0 mL
0.2-8.7 20.0 10.0 25.0 mL
0.8-35 10.0 5.00 25.0 mL
8-350 5.00 1.00 25.0 mL
80-3500 1.00 0.50 25.0 mL
A × 2500
------------------------ = mg/L Total Mn
B× C
47
Nickel, PAN (Method 8150)
Expected Ni Sample Analysis

Dilute to
0.05-3 40.0 20.0 25.0 mL
0.2-12 20.0 10.0 25.0 mL
0.8-47 10.0 5.00 25.0 mL
8-470 5.00 1.00 25.0 mL
80-4700 1.00 0.50 25.0 mL
A × 2500- = mg/L Total Ni

-----------------------
B× C
Nitrogen TKN (Method 8075)
Expected
Sample Analysis
Nitrogen Dilute to
amount (mL) Volume (mL)
conc. (mg/L)
0.5-28 40.0 10.0* 25.0 mL*
2-112 20.0 5.00* 25.0 mL*
11-560 10.0 2.00* 25.0 mL*
45-2250 5.00 1.00* 25.0 mL*
425-22500 1.00 0.50* 25.0 mL*
*These are guidelines only. See the spectrophotometer procedure manual.
A × 75
----------------- = mg/L TKN
B× C
48
Phosphorus, Ascorbic Acid (Method 8048)
Expected PO4 Sample Analysis

Dilute to
0.12-6 40.0 20.0 25.0 mL

0.5-23 20.0 10.0 25.0 mL
2-90 10.0 5.00 25.0 mL
20-900 5.00 1.00 25.0 mL
200-9000 1.00 0.50 25.0 mL
A × 2500
------------------------ = mg/L Total PO4
B× C
Potassium (Method 8049)
Expected K Sample Analysis

Dilute to
4-20 40.0 20.0 25.0 mL
15-80 20.0 10.0 25.0 mL
60-300 10.0 5.00 25.0 mL
200-1000 5.0 3.00 25.0 mL
600-3000 5.00 1.00 25.0 mL
2000-10000 3.0 0.500 25.0 mL
6000-30000 1.00 0.50 25.0 mL
A × 2500- = mg/L Total K

-----------------------
B× C
49
Silver (Method 8120)
Expected Ag Sample Analysis

Dilute to
0.08-3.7 40.0 20.0 50.0 mL
0.3-15 20.0 10.0 50.0 mL
1.0-60 10.0 5.00 50.0 mL
12-600 5.00 1.00 50.0 mL
120-6000 1.00 0.50 50.0 mL
A × 5000- = mg/L Total Ag

-----------------------
B× C
Zinc (Method 8009)
Expected Zn Sample Analysis

Dilute to
0.2-12.5 40.0 20.0 50.0 mL
0.8-50 20.0 10.0 50.0 mL
3.0-200 10.0 5.00 50.0 mL
30-2000 5.00 1.00 50.0 mL
300-20000 1.00 0.50 50.0 mL
A × 5000
------------------------ = mg/L Total Zn
B× C
50
51
Danger
Danger
52
DIGESTION PROCEDURE FOR OILS
1. Transfer 0.25 g or 2. Add 4 mL 3. Turn the temperature 4. Place the flask weight
less of sample into a concentrated sulfuric dial to a heat setting of followed by the
100-mL Digesdahl acid (spec. gravity 1.84) 440 ° C (825 ° F). When fractionating column
digestion flask; see to the digestion flask. the proper temperature is with funnel on the flask.
Sample and Analysis Note: Use only Hach reached, turn on the Place the flask on the
Volume Tables for Oils Digesdahl digestion flasks. water to the aspirator heater and boil 4
following this Volumetric flasks with and make sure there is minutes. Do not boil to
procedure. concave bottom should not suction to the dryness! If sulfuric acid
be used. fractionating column. is not present in the
Note: Take care to
ensure you have a Note: Safety glasses and Note: Wait for the proper flask after the boiling
homogenous sample. a safety shield placed temperature to be reached period, do not proceed
between the operator and before sample is placed on to Step 5! Discard the
the Digesdahl are required. the heater. sample and use more
sulfuric acid for the
digestion procedure in
Step 2. Or choose a
smaller sample size for
digestion from the
Sample and Analysis
Volume Tables for Oils,
following this procedure.
lower temperature to
335 ° C (635 ° F). Continue
heating at lower
temperature until all
water is evaporated. Then
return to original
digestion temperature.
53
DIGESTION PROCEDURE FOR OILS, continued
5. Do not proceed if 6. After addition of 7. Take the hot flask off 8. Dilute the digest
sulfuric acid is not visible hydrogen peroxide is the heater and allow the to approximately 70 mL
in the flask. Add 10 mL complete, boil off excess flask to air cool. Remove with deionized water.
of 50% hydrogen hydrogen peroxide by the fractionating column Note: Add demineralized
peroxide to the charred heating for one more from the digestion flask. water slowly at first. Cool
sample via the funnel on minute. Do not heat Note: Use finger cots to the flask if necessary
the fractionating head. to dryness. remove the digestion flask. for handling.
Note: Visually confirm the Note: If the sample goes to Place it on a cooling pad
presence of sulfuric acid in dryness, turn off the for at least one minute.
the flask before adding Digesdahl and air cool Then remove the column.
hydrogen peroxide. completely. Add water Do not add water to the
to flask before handling. flask until it has cooled.
Note: If the digest does not
turn colorless, add 5 mL Repeat digestion from the
increments of peroxide until beginning using a new
the digest becomes clear or sample.
does not change color.
during hydrogen peroxide
addition, stop the peroxide
flow and remove the
digestion flask and
fractionating column (use
finger cots). Cool for
30 seconds and return
apparatus to the heating
block. Start peroxide
addition with 2 mL,
then follow with the
remaining peroxide.
54
9. If analyzing for 10. Turn the 11. If the sample is 12. Continue the
aluminum, nickel or temperature dial to a visibly turbidity, filter or analysis using the
iron, continue to Step heat setting of 204 ° C wait until the turbidity appropriate procedure
10. If analyzing for other (400 ° F). Add 150 mL of settles, and the upper below.
substances, dilute to the water to a 400-mL portion of the sample is
100-mL mark with beaker. Place the beaker clear.
deionized water; Skip on the heater. Place the Filter as follows:
Step 10 and go to flask in the beaker and
Step 11. boil for15 minutes. Cool a) Place a filter paper into
to room temperature and
dilute
to the mark with b) Place the filter holder
demineralized water. assembly in the filtering
flask and wet the filter
Invert several times
with demineralized water
to mix.
to ensure adhesion to
Note: When using a the holder.
Digesdahl Digestion
Apparatus system without c) While applying a
temperature control dials, vacuum to the filtering
reset to a lower setting that flask, transfer the sample to
gently boils the water. the filtering apparatus.
another container.
Metals Method

graduate cylinder. See Sample and Analysis Volume Tables for Oils
following the specific digestion to determine the analysis volume.
graduated cylinder.
55
instead.

Note: High iron content will cause precipitation (brown cloud) which will co-precipitate
other metals. Repeat this procedure with a smaller aliquot volume.

are analyzing.

not available.

times to mix.
color appears.
56
6. Add deionized water to the volume indicated in the
colorimetric procedure.
Sample and Analysis Volume Tables for Oils


conc. (mg/kg) amount (g) Volume (mL)
15-800 0.250 20.0
40-2000 0.200 10.0
100-5300 0.150 5.00
1000-40000 0.100 1.00
A × 5000
------------------------ = mg/kg Total Al
B× C
B = g sample amount from table

7-220 0.250 20.0
20-550 0.200 10.0
50-1400 0.150 5.00
400-11000 0.100 1.00
A × 5000
------------------------ = mg/kg Total Al
B× C
57

10-400 0.250 20.0
25-1000 0.200 10.0
65-2600 0.150 5.00
480-20000 0.100 1.00
A × 25
----------------- = mg/kg Total Cd
B× C
A = µg/l reading from instrument
Chromium, Total (Method 8024)

8-300 0.250 20.0
20-750 0.200 10.0
50-2000 0.150 5.00
350-15000 0.100 1.00
A × 2500- = mg/kg Total Cr

-----------------------
B× C
58

15-950 0.250 20.0
45-2400 0.200 10.0
120-6200 0.150 5.00
880-46000 0.100 1.00
A × 2500
------------------------ = mg/kg Total Co
B× C

40-2300 0.250 20.0
100-6000 0.200 10.0
320-15000 0.150 5.00
2000-110000 0.100 1.00
A × 2500- = mg/kg Total Cu

-----------------------
B× C
59

25-1400 0.250 20.0
60-3500 0.200 10.0
160-9300 0.150 5.00
1200-70000 0.100 1.00
A × 2500
------------------------ = mg/kg Total Fe
B× C

11-650 0.250 20.0
30-1600 0.200 10.0
75-4300 0.150 5.00
560-32000 0.100 1.00
A × 2500- = mg/kg Total Fe

-----------------------
B× C
60

15-800 0.250 20.0
38-2000 0.200 10.0
100-5300 0.150 5.00
750-40000 0.100 1.00
A × 25
----------------- = mg/kg Total Pb
B× C

7-350 0.250 20.0
20-870 0.200 10.0
50-2300 0.150 5.00
400-17000 0.100 1.00
A × 2500- = mg/kg Total Mn

-----------------------
B× C
61

7-470 0.250 20.0
20-1200 0.200 10.0
50-3100 0.150 5.00
350-23000 0.100 1.00
A × 2500
------------------------ = mg/kg Total Ni
B× C
Expected Nitrogen Sample Analysis

85-4500 0.250 10.0*
210-11000 0.200 5.00*
2100-110000 0.100 1.00*
A × 75
----------------- = mg/kg TKN
B× C
62

20-900 0.250 20.0

50-2300 0.200 10.0
130-6200 0.150 5.00
1000-45000 0.100 1.00
A × 2500
------------------------ = mg/kg Total PO4
B× C

600-3400 0.250 20.0
1500-8500 0.200 10.0
4100-22000 0.150 5.00
15500-85000 0.100 2.00
31000-170000 0.100 1.00
A × 2500- = mg/kg Total K

-----------------------
B× C
63

12-600 0.250 20.0
30-1500 0.200 10.0
80-4000 0.150 5.00
620-30000 0.100 1.00
A × 5000
------------------------ = mg/kg Total Ag
B× C
Zinc (Method 8009)

30-2000 0.250 20.0
80-5000 0.200 10.0
200-13000 0.150 5.00
1600-100000 0.100 1.00
A × 5000- = mg/kg Total Zn

-----------------------
B× C
64
65
Danger
Danger
66
DIGESTION PROCEDURE FOR SOLIDS
1. Transfer 0.50 g or 2. Add 4 mL 3. Turn the temperature 4. Place the flask weight
less of sample into a concentrated sulfuric dial to a heat setting of followed by the
100-mL Digesdahl acid (spec. gravity 1.84) 440 ° C (825 ° F). When fractionating column
digestion flask; see to the digestion flask. the proper temperature is with funnel on the flask.
Sample and Analysis Note: Use only Hach reached, turn on the Place the flask on the
Volume Tables for Digesdahl digestion flasks. water to the aspirator heater and boil 4
Solids following Volumetric flasks with and make sure there is minutes. Do not boil to
this procedure. concave bottom should not suction to the dryness! If sulfuric acid
be used. fractionating column. is not present in the
Note: Be sure you have a
homogenous sample. Solid Note: Safety glasses and a Note: Wait for the proper flask after the boiling
sample should be finely safety shield placed temperature to be reached period, do not proceed
ground or chopped and between the operator and before sample is placed on to Step 5! Discard the
mixed well. the Digesdahl are required. the heater. sample and use more
sulfuric acid for the
digestion procedure in
Step 2. Or choose a
smaller amount from the
Sample and Analysis
Volume Tables for
Solids.
lower temperature to
335 ° C (635 ° F). Continue
heating at lower
temperature until all
water is evaporated. Then
return to original
digestion temperature.
Note: White acid vapors
accompanied with a reflux
line indicate that the
sulfuric acid is boiling
Note: Some organic
samples may need more
than 5 minutes for
complete digestion.
67
DIGESTION PROCEDURE FOR SOLIDS, continued
5. Do not proceed if 6. After addition of 7. Take the hot flask off 8. Dilute the digest to
sulfuric acid is not hydrogen peroxide is the heater and allow the approximately 70 mL
visible in the flask. Add complete, boil off excess flask to air cool. with deionized water.
10 mL of 50% hydrogen hydrogen peroxide by Remove the Note: Add deionized
peroxide to the charred heating for one more fractionating column water slowly at first. Cool
sample via the funnel on minute . Do not heat to from the digestion flask. the flask if necessary
the fractionating dryness. Note: Use finger cots to for handling.
column. Note: If the sample goes to remove the digestion flask.
Note: Do not heat to dryness. dryness, turn off the Place it on a cooling pad
for at least one minute.
Note: Visually confirm the Digesdahl and air cool to
Then remove the column.
presence of sulfuric acid in room temperature. Add
water to flask before Do not add water to the
the flask before adding
handling. Repeat the flask until it has cooled.
hydrogen peroxide.
digestion from the
Note: If the digest does not beginning using a new
turn colorless, add 5 mL sample.
increments of peroxide until
the digest becomes clear or
does not change color.
during hydrogen peroxide
addition, stop the peroxide
flow and remove the
digestion flask and
fractionating column
(use finger cots). Cool for
30 seconds and return
apparatus to the heating
block. Start peroxide
addition with 2 mL,
then follow with the
remaining peroxide.
68
9. If analyzing for 10. Turn the temperature 11. If the sample has 12. Continue with the
aluminum, nickel or dial to a heat setting of visible turbidity, filter or analysis using the
iron, continue to Step 204 ° C (400 ° F). Add wait until the turbidity appropriate procedure
10. If analyzing for other 150 mL of water to a settles, and the upper below.
substances, dilute to the 400-mL beaker. Place portion of the sample
100-mL mark with the beaker on the heater. is clear.
deionized water; skip Place the flask in the Filter as follows:
Step 10 and go to beaker and boil for 15
a) Place a filter paper into
Step 11. minutes. Air cool to
room temperature and wrinkled surface upward.
dilute to the mark with
deionized water. Invert b) Place the filter holder
assembly in the filtering
several times to mix.
flask and wet the filter
Note: When using a with deionized water to
Digesdahl Digestion ensure adhesion to
Apparatus system without the holder.
temperature control dials,
reset to a lower setting that c) While applying a
gently boils the water. vacuum to the filtering
another container.
Note: If small aliquots
(≤1.0 mL) are analyzed,
filtration is not needed.
Metals Method

graduate cylinder. See Sample and Analysis Volume Tables for Solids
following the specific digestion to determine the analysis volume.
graduate cylinder.
69
instead.

Note: High iron content will cause precipitation (brown cloud) which will co-precipitate
other metals. Repeat this procedure with a smaller aliquot volume.

are analyzing.

not available.

times to mix.
color appears.
70
procedure.
Sample and Analysis Volume Tables for Solids


10-400 0.500 20.0
25-1000 0.400 10.0
65-2600 0.300 5.00
480-20000 0.200 1.00
1900-80000 0.100 0.50
A × 5000
------------------------ = mg/kg Total Al
B× C

4-100 0.500 20.0
10-270 0.400 10.0
25-730 0.300 5.00
180-5500 0.200 1.00
750-22000 0.100 0.50
A × 5000
------------------------ = mg/kg Total Al
B× C
71

5-200 0.500 20.0
12-500 0.400 10.0
30-1300 0.300 5.00
240-10000 0.200 1.00
960-40000 0.100 0.50
A × 25 = mg/kg Total Cd
-----------------
B× C
Chromium, Total (method 8024)

4.9-150 0.500 20.0
10-370 0.400 10.0
25-1000 0.300 5.00
190-7500 0.200 1.00
750-30000 0.100 0.50
A × 2500
------------------------ = mg/kg Total Cr
B× C
72

10-450 0.500 20.0
20-1200 0.400 10.0
50-3000 0.300 5.00
500-20000 0.200 1.00
2000-100000 0.100 0.50
A × 2500- = mg/kg Total Co

-----------------------
B× C

20-1200 0.500 20.0
50-3000 0.400 10.0
120-7500 0.300 5.00
1000-60000 0.200 1.00
4000-240000 0.100 0.50
A × 2500
------------------------ = mg/kg Total Cu
B× C
73

12-700 0.500 20.0
35-1700 0.400 10.0
85-4500 0.300 5.00
650-35000 0.200 1.00
2500-140000 0.100 0.50
A × 2500- = mg/kg Total Fe

-----------------------
B× C

6-300 0.500 20.0
15-800 0.400 10.0
40-2000 0.300 5.00
300-15000 0.200 1.00
1200-65000 0.100 0.50
A × 2500
------------------------ = mg/kg Total Fe
B× C
74

8-400 0.500 20.0
20-1000 0.400 10.0
50-2600 0.300 5.00
400-20000 0.200 1.00
1500-80000 0.100 0.50
A × 25 = mg/kg Total Pb
-----------------
B× C

4-170 0.500 20.0
10-430 0.400 10.0
25-1100 0.300 5.00
200-8700 0.200 1.00
750-35000 0.100 0.50
A × 2500
------------------------ = mg/kg total Mn
B× C
75

4-220 0.500 20.0
10-580 0.400 10.0
25-1500 0.300 5.00
200-11000 0.200 1.00
750-45000 0.100 0.50
A × 2500- = mg/kg Total Ni

-----------------------
B× C
Expected Nitrogen Sample Analysis

42-2200 0.500* 10.0*
106-5600 0.400* 5.00*
350-18000 0.300* 2.00*
1000-56000 0.200* 1.00*
4200-220000 0.100* 0.50*
A × 75
----------------- = mg/kg TKN
B× C
76

10-450 0.500 20.0

25-1100 0.400 10.0
67-3100 0.300 5.00
500-23000 0.200 1.00
2000-93000 0.100 0.50
A × 2500
------------------------ = mg/kg Total PO4
B× C

300-1700 0.500 20.0
800-4200 0.400 10.0
2000-11000 0.300 5.00
15000-85000 0.200 1.00
62000-300000 0.100 0.50
A × 2500
------------------------ = mg/kg Total K
B× C
77

6-300 0.500 20.0
15-750 0.400 10.0
40-2000 0.300 5.0
300-15000 0.200 1.00
1200-60000 0.100 0.50
A × 5000- = mg/kg Total Ag

-----------------------
B× C
Zinc (Method 8009)

16-1000 0.500 20.0
40-2500 0.400 10.0
100-6600 0.300 5.00
800-50000 0.200 1.00
3000-200000 0.100 0.50
A × 5000
------------------------ – mg/kg Total Zn
B× C
78
MAINTENANCE
Some of the following manual sections contain warning

labels and require special attention.
Read and follow all warning instructions carefully to avoid

personal injury and damage to the instrument. Only
qualified personnel should conduct maintenance
procedures on this instrument.
79
80
SECTION 5 MAINTENANCE
5.1 Fuse Replacement
The fuse holder is located on the back panel within the power cord
receptacle. See Figure 2. To replace a fuse, turn off the instrument power
and disconnect the power cord from the back panel. Removal of the
vertical support is necessary. Remove the fuse holder by prying with a
small screwdriver or other pointed tool at the small opening at the top of
the fuse holder. Replace the fuse with the same type and rating used
originally. Refer to Replacement Parts.
5.2 Kit Replacement Parts

Description Unit Cat. No.
Aspirator, without check valve, 3/8” NPT ..................................................each ............2131-02
Cooling Pad .................................................................................................each ..........18376-00
Finger Cots ................................................................................................pkg/2 ..........14647-02
Flask, digestion, 100 mL .............................................................................each ..........23125-42
Flask Weight................................................................................................each ..........44340-00
Fractionating Head ......................................................................................each ..........22855-20
Fractionating Column Kit..............................................................................................23131-20
Kit includes: Fractionating Head; Capillary Flow Funnel 8.3 cm
(3.25”); Column Baffle; Tubing; C-Flex, 5 feet; Vent Trap Body; and
Vent Trap Cap
Funnel, Capillary Flow................................................................................each ..........22856-00
Fuse, 4 A, 125 V Slow-blow, for heater assembly ......................................each ..........44591-00
Fuse, 2 A, for 250 V heater assembly .........................................................each ..........44398-00
Goggles, safety ............................................................................................each ..........18421-00
Heat Shield ..................................................................................................each ..........18380-00
Heater Assembly, 115 V..............................................................................each ..........44336-20
Heater Assembly, 230 V..............................................................................each ..........44336-21
Heater Element Assembly, 120 V ...............................................................each ..........18565-01
Heater Element Assembly, 240 V ...............................................................each ..........18565-02
Instruction Manual ......................................................................................each ..........23130-18
Power Cord, 115 V, UL/CSA approved ......................................................each ..........18010-00
Power Cord, 230V, VDE-approved for European operation .......................each ..........46836-00
Receptacle, column .....................................................................................each ..........45926-00
Tubing, C-flex ........................................................................................ 25 feet ..........23273-37
Vertical Support, heater ...............................................................................each ..........44378-00
81
82
GENERAL INFORMATION
At Hach Company, customer service is an

important part of every product we make.
With that in mind, we have compiled the following

information for your convenience.
83
84
REPLACEMENT PARTS
REQUIRED REAGENTS
Quantity Required
Description Per Digestion Unit Cat. No.
Hydrogen Peroxide, 50% ................................................... 10 mL .......... 500 mL .......21196-49
Sulfuric Acid, ACS,
(concentrated, spec. gravity 1.84).............................. ≥ 2.5 mL .............. 4 kg ...........979-09
Water, demineralized ...........................................................varies...................4 L ...........272-56
REQUIRED APPARATUS
Dispenser, pour-out, 10 mL.................................................... 1.....................each .......22200-38
Pipet, serological, 10 mL........................................................ 1.....................each ...........532-38
Pipet filler, safety bulb ........................................................... 1.....................each .......14651-00
Boiling chips, silicon carbide ..............................................varies............... 500 g .......20557-34
Safety glasses ......................................................................... 1.....................each .......18421-00
Safety shield, for Digesdahl ................................................... 1.....................each .......20974-00
Select one based on available voltage:

Digesdahl Apparatus, 115 Vac .......................................................................each .......23130-20
Digesdahl Apparatus, 230 Vac .......................................................................each .......23130-21
OPTIONAL REAGENTS
Hydrogen Peroxide, 30% ......................................................................... 200 mL ...........144-45
Kjeldahl Reduction Reagent (for fluid fertilizers) ......................................... 40 g .......23653-04
2, 4-Dinitrophenol Indicator Solution ............................................ 100 mL MDB .........1348-32
Nitric Acid Solution, 1:1 .......................................................................... 500 mL .........2540-49
Potassium Hydroxide, 1 N .............................................................. 50 mL SCDB .......23144-26
Potassium Hydroxide Standard Sol’n, 8 N............................................... 500 mL ...........282-49
Sodium Hydroxide, 5 N ................................................................ 50 mL* SCDB .........2450-26
Sodium Hydroxide, 1 N ............................................................... 118 mL* MDB .........1045-37
TKN Indicator Solution................................................................... 50 mL SCDB .......22519-26
OPTIONAL APPARATUS
Balance, Precision, 115 V ..............................................................................each .......26104-00
Balance, Precision, 230 V ..............................................................................each .......26104-02
Beaker, 400 mL ..............................................................................................each ...........500-48
Beaker, Berzelius, 200 mL .........................................................................12/pkg .......22761-75
Bottle, Wash, 1 L............................................................................................each ...........620-16
Bulb, dropper, 2 mL ...................................................................................12/pkg .......21189-00
Cylinder, graduated, 50 mL............................................................................each ...........508-41
Dispenser, 1-5 mL (for H2SO4, meat)............................................................each .......23121-37
Dispenser, 10-50 mL (for H2SO4, meat)........................................................each .......23121-41
Filter discs, glass, 47 mm .........................................................................100/pkg .........2530-00
Filter holder, membrane .................................................................................each .........2340-00
85
REPLACEMENT PARTS, continued
OPTIONAL APPARATUS (continued)
Flask, filter, 500 mL....................................................................................... each........... 546-49
Flask, flat-bottom volumetric, 100 mL .......................................................... each....... 23125-42
Fume Scrubber Apparatus, 115 V.................................................................. each....... 23266-00
Fume Scrubber Apparatus, 230 V.................................................................. each....... 23266-02
Oven, laboratory, 120 V................................................................................. each....... 14289-00
Oven, laboratory, 230V.................................................................................. each....... 14289-02
Paper, weighing, 76 x 76 mm .................................................................. 500/pkg....... 14738-00
pH paper, pH 1-11..................................................................................5 roll/pkg........... 391-33
Pipet, Pasteur, disposable, 229 mm.......................................................... 200/pkg....... 21234-01
sension™1 Basic Portable pH Meter, with electrode ................................... each....... 51700-10
Spatula, stainless, 10 cm ................................................................................ each........... 561-64
Spoon, measuring, 0.05 g............................................................................... each........... 492-00
Stir bar, PTFE, 1”........................................................................................... each....... 20953-51
Stir plate, magnetic, 7X7, 115 Vac................................................................. each....... 23444-00
Stir plate, magnetic, 7X7, 230 Vac................................................................. each....... 23444-02
Stopper, hollow, size #5 ............................................................................... 6/pkg....... 14480-05
Syringe, 5 mL, plastic .............................................................................. 100/pkg....... 23433-33
Watch Glass, 65 mm .................................................................................. 12/pkg........... 578-97
86
HOW TO ORDER
87
REPAIR SERVICE
88
WARRANTY
89

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23130-18

AccuGrow® H2OU™ PourRite™

Hach Company certifies this instrument was tested thoroughly, inspected

SECTION 1 GENERAL DESCRIPTION ............................................................................ 3

SECTION 2 PREPARATION FOR USE .............................................................................. 5

SECTION 3 SAFETY & ENVIRONMENTAL CONSIDERATIONS............................. 11

SECTION 4 OPERATION ................................................................................................... 21

4.2.7 Sampling and Storage.............................................................................................. 25

DIGESTION PROCEDURE FOR AQUEOUS LIQUIDS................................................. 39

DIGESTION PROCEDURE FOR OILS............................................................................. 53

DIGESTION PROCEDURE FOR SOLIDS ....................................................................... 67

Pay particular attention to Section 3! Failure to do so could result in

Use of Danger Messages, Cautions and Notes

Personal injury or damage to the instrument could occur if not observed.

This symbol, if noted on the instrument, references the Instruction

3.1 Digesdahl Digestion Apparatus

3.2 Using Hydrogen Peroxide

3.3 Using Sulfuric Acid

3.4 Clean Up of Spills and Leaks

Digestion takes a fraction of the time required for traditional methods.

1.2 Scope of Instructions

Verify that the following items are present:

• Heater Assembly, with power cord, fuse

1. Place the fractionating column in the column receptacle (shown in

3. Place the vent trap cap on the capillary funnel adapter .

3.1 Digesdahl Digestion Apparatus

• Sample size -- Never digest a sample which contains over 0.5 g of

• Oils and organic liquids should be considered as solids when

• Acid type -- Only use acid specified in Hach step-by-step procedures.

• Always perform digestion behind a safety shield (Cat. No. 20974-00) or in

• For respiratory protection, use a fume hood or Hach’s Fume Scrubber

• Do not add alcohol, acetone or other organic solvents to the digestion

• Use laboratory coats or aprons to protect skin and clothing

• Wear appropriate shoes to protect feet from spills. Open-toed shoes

• Do not use damaged glassware or apparatus. Discard all damaged

3.2 Using Hydrogen Peroxide

Use these additional specific safety precautions when using hydrogen

• Do not mix hydrogen peroxide with any chemical reagents except as

• Do not add hydrogen peroxide directly to the column on the digestion

• Hydrogen peroxide should be added to the organic materials in the

• Do not use hydrogen peroxide in concentrations greater than 50%.

Hydrogen peroxide is highly corrosive and should be cleaned up with

• It is a strong oxidizing agent. The chemical nature of hydrogen

• It can decompose, releasing heat and oxygen. Normally this rate is

Please observe the following precautions for handling and storing of

• Do store in a cool place away from direct sunlight (preferably in

• Do store in the original containers with closures as supplied and keep

• Do wear gloves and safety glasses when handling the material.

• Do wash eyes with plenty of water if contaminated and get medical

• Do get medical advice without delay if the material is ingested.

• Do not inhale vapors or ingest the material.

3.3 Using Sulfuric Acid

Concentrated sulfuric acid used in the digestion process should be

Sulfuric acid mist or vapor has been classified by the International

Sulfuric acid is a strong oxidizer. It may ignite or explode on contact with

3.4 Clean Up of Spills and Leaks

A spill, overflow, or eruption from the Digesdahl apparatus may leave a

3.5 Waste Management

Section 3 summarizes basic requirements for safely handling the

For further information, please contact the Hach Environmental Safety

3.6 Minéralisateur Digesdahl

• Poids d’échantillon : Ne jamais minéraliser un échantillon qui contient

• Les huiles et liquides organiques doivent être considérés comme des