Digesdahl® Digestion Apparatus Models 23130-20, Manual

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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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 610101 (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 TV 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 TV Product Services, certified compliance by Hach Company. This Class A digital apparatus meets all requirements of the Canadian Interference- Causing Equipment Regulations. Cet appareil numrique de la classe A respecte toutes les exigences du Rglement sur le matriel brouilleur du Canada. FCC Part 15, Class "A" Limits: Supporting test records by TV 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 .............................................................................. 2.1 Unpacking ........................................................................................................................... 2.2 Assembly............................................................................................................................. 2.2.1 Heater Assembly........................................................................................................ 2.2.2 Fractionating Head System........................................................................................ 2.3 Selecting a Temperature Setting.......................................................................................... SECTION 3 SAFETY & ENVIRONMENTAL CONSIDERATIONS ............................. 3.1 Digesdahl Digestion Apparatus......................................................................................... 3.2 Using Hydrogen Peroxide ................................................................................................. 3.3 Using Sulfuric Acid........................................................................................................... 3.4 Clean Up of Spills and Leaks............................................................................................ 3.5 Waste Management ........................................................................................................... CONSIDERATIONS DE SECURITE ET DENVIRONNEMENT....................................... 3.6 Minralisateur Digesdahl .................................................................................................. 3.7 Utilisation de leau oxygne............................................................................................ 3.8 Utilisation de lacide sulfurique ........................................................................................ 3.9 Nettoyage des dversements et fuites................................................................................ SECTION 4 OPERATION ................................................................................................... 4.1 Apparatus Preparation ....................................................................................................... 4.2 Digestion ........................................................................................................................... 4.2.1 Appropriate Sample Size ......................................................................................... 4.2.2 Proper Digestion Solution Temperature .................................................................. 4.2.3 Sufficient Sulfuric Acid ........................................................................................... 4.2.4 Carbonization Period ............................................................................................... 4.2.5 Adequate Peroxide Concentration for Sufficient Time............................................ 4.2.6 Containment of Sample ........................................................................................... v 5 5 6 6 7 9
11 11 12 14 14 15 16 16 17 19 20 21 21 21 22 22 22 24 24 25
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 chantillons chimiques, talons et ractifs peut tre dangereuse. Lire les fiches de donnes de scurit des produits ncessaires et se familiariser avec toutes les procdures de scurit avant de manipuler tout produit chimique.
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 na pas de protection contre la surchauffe lorquil est utilis sur une alimentation lectrique en triphas. Utiliser cet appareil seulement sur alimentation 230 V monophas.
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.
Figure 1 Digesdahl Digestion Apparatus
CAPILLARY FUNNEL VENT TRAP CAP CAPILLARY FUNNEL ADAPTOR
VENT TRAP BODY
COLLUMN BAFFLE FRACTIONATING COLUMN
COLUMN RECEPTACLE SAFETY SHIELD
VERTICAL SUPPORT
HEAT SHIELD
FLASK WEIGHT DIGESTION FLASK
TEMPERATURE INDICATOR
TEMPERATURE CONTROL
POWER SWITCH MODE SWITCH
HEATER ASSEMBLY
SECTION 2
2.1 Unpacking
PREPARATION FOR USE
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.
2.2
Assembly
2.2.1 Heater Assembly Assemble the heater assembly as shown in Figure 2.
Figure 2 Heater Assembly
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'purateur de fumes Hach peut seulement tre utilis avec le minralisateur Digesdahl pour des minralisarions l'acide sulfurique. Des conditions de risque peuvent tre cres par l'aspiration de vapeurs d'un autre acide dans l'purateur de fumes. Il est important de nettoyer l'purateur de fumes aprs chaque utilisation pour viter 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
2.3
Selecting a Temperature Setting

The particular temperature applicable for the sample to be digested is given in the appropriate analysis procedure manual. The steps below explain how to set the heater temperature. 1. Connect the power cord to the line voltage receptacle and set the POWER switch to ON. The TEMPERATURE indicator will light. 2. Set the Mode switch to SET. The TEMPERATURE indicator will display the current temperature set point in degrees Celsius. 3. If a different temperature is desired, adjust the Temperature ADJ control for the desired temperature in the digital display. 4. Set the Mode switch to READ and allow time (approximately 10 minutes) for the heater to reach the selected temperature. With the Mode switch in the READ position, the temperature display shows the current operating temperature.
Note: During a digestion, the temperature reading will vary slightly above and below the selected temperature. This will not affect the digestion or the accuracy of the final analysis. When idling (no digestion flask in place), the temperature may fluctuate 15 C from the set point.
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 Digesdahls 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 Hachs 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 generators 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.
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CONSIDERATIONS DE SECURITE ET DENVIRONNEMENT

Chaque personne effectuant des analyses de laboratoire est responsable de la scurit. Lanalyste doit dvelopper et appliquer de bonnes habitudes de scurit pour minimiser les risques daccidents en pratiquant de bonnes techniques de laboratoire.
3.6
Minralisateur Digesdahl
Pour une utilisation du Digesdahl en toute scurit, observer les prcautions suivantes :
Poids dchantillon : Ne jamais minraliser un chantillon qui contient

plus de 0,5 g de produit qui ne soit pas de leau.
Les huiles et liquides organiques doivent tre considrs comme des

solides pour la dtermination du poids dchantillon.
Type dacide : Utiliser seulement lacide spcifi dans les techniques

dtailles de Hach.
Volume dacide : Ne jamais utiliser moins de 3 ml. Toujours suivre lordre des oprations indiqu. Si la fiole va sec, la retirer immdiatement du systme de chauffage
et la laisser refroidir la temprature ambiante. Ne jamais ajouter deau oxygne une fiole dchantillon sec, une explosion pourrait se produire. Si vous ntes pas sr que la fiole contienne assez dacide sulfurique, ARRETEZ. Ne pas ajouter deau oxygne. Recommencer lopration avec une quantit dchantillon plus petite ou plus dacide.
Prendre soin de maintenir en place la chemine et le manchon de

scurit du Digesdahl pendant lutilisation.
Toujours effectuer les minralisations derrire un cran de protection

(# 20974-00) ou sous une hotte ferme.
Pour une protection respiratoire, utiliser une hotte ou lpurateur de

fumes Hach (rf. n 23266).
Toujours porter des lunettes de scurit avec protections latrales. Porter des gants pour la protection pendant les oprations de digestion.
Utiliser des pinces ou des doigtiers de protection pour dplacer les objets chauds.
16
NE PAS ajouter dalcool, dactone ou autre solvant organique dans la

fiole de digestion avant ou aprs minralisation.
Pendant la digestion, utiliser le rglage de temprature et le temps de

digestion spcifi dans les instructions. Ne pas laisser le Digesdahl sans surveillance pendant lutilisation.
Lors de la minralisation dune nouvelle substance pour la premire

fois, commencer avec une quantit plus petite avant dutiliser la quantit optimale pour lanalyse. Ne pas laisser le contenu de la fiole svaporer sec.
Porter une blouse ou un tablier de laboratoire pour protger la peau et

les vtements des projections.
Porter des chaussures appropries pour protger les pieds des

dversements de produits. Ne pas porter de chaussures bout ouvert.
Ne pas utiliser de verrerie ou appareils endommags. Eliminer et

remplacer tous les quipements endommags.
Laisser le Digesdahl refroidir naturellement (dans lair ambiant). Leau

froide peut briser le verre chaud.
3.7
Utilisation de leau oxygne

Utilisez ces prcautions de scurit supplmentaires spcifiques pour lutilisation de leau oxygne dans les minralisations par le Digesdahl :
DANGER Leau oxygne (peroxyde dhydrogne) sous forme concentre prsente un risque dexplosion.
NE PAS mlanger leau oxygne avec dautres ractifs sauf

indication prcise dans les procdures danalyse Hach.
NE PAS ajouter deau oxygne directement dans la colonne de

fractionnement sur la fiole de digestion. Ajouter toujours leau oxygne avec un dbit lent et rgulier, utiliser lentonnoir capillaire Hach.
Leau oxygne doit tre ajoute la matire organique carbonise

dans la fiole, seulement en prsence dacide sulfurique.
NE PAS utiliser deau oxygne des concentrations suprieures

50%.
17
Leau oxygne (30% ou 50%) est un oxydant puissant et ne doit jamais tre stock prs de matires inflammables. Comme lacide sulfurique, il peut provoquer des brlures la peau et aux yeux. En cas de contact avec les yeux ou la peau, laver les yeux et/ou la peau leau pendant 15 minutes. Retirer les vtements contamins. Appeler un mdecin. Leau oxygne est extrmement corrosive et doit tre lave leau si elle est rpandue sur des appareils ou sur la paillasse. Lire et observer tous les avertissements sur les tiquettes des ractifs et les fiches de donnes de scurit des produits. Les procdures de manipulations et de stockage concernant leau oxygne doivent tenir compte de deux caractristiques importantes du produit :
Cest un agent fortement oxydant. La nature chimique de leau

oxygne en fait un produit irritant pour la peau, les muqueuses et particulirement les yeux. Il provoque des brlures graves aux concentrations auxquelles il est utilis dans lindustrie et peut provoquer une combustion spontane au contact immdiat ou prolong des combustibles.
Il peut se dcomposer avec dgagement de chaleur et doxygne. La

vitesse de dcomposition naturelle du produit de qualit industrielle courante est trs lente, mais elle sacclre lorsquelle est contamine par des substances telles que poussire, ions mtalliques, ou alcalines. Prendre les prcautions suivantes pour la manipulation et le stockage de leau oxygne :
Stocker dans un endroit frais labri de la lumire directe du soleil

(de prfrence dans un rfrigrateur).
Stocker dans les rcipients dorigine avec les bouchons fournis et les
maintenir ferms lorsquils ne sont pas utiliss. (Sassurer que les rcipients sont ventils. Les flacons deau oxygne Hach sont livrs avec un joint de bouchon permable spcial).
Porter des gants et des lunettes de scurit lors de la manipulation

du produit.
Utiliser des grains de carbure de silicium pour rgulariser lbullition

lors de la digestion dchantillons liquides.
18
Laver la peau contamine rapidement grande eau. Retirer rapidement

les vtements contamins et les laver soigneusement avant de les rutiliser. Les laver rgulirement.
Laver les yeux grande eau sils sont contamins et consulter un

mdecin immdiatement.
Consulter immdiatement un mdecin si le produit est ingr. Laver toute trace rpandue grande eau. NE PAS stocker prs des sources de chaleur ou au contact de
combustibles ou de produits organiques.
NE PAS laisser le produit stock ou enferm dans un espace clos. NE PAS inhaler les vapeurs ou ingrer le produit. NE PAS mettre le produit au contact des yeux et de la peau. NE PAS laisser au contact avec des catalyseurs de dcomposition
(mtaux, poussires, produits alcalins, etc.).
NE PAS utiliser de matriaux de construction inadapts (laiton,

cuivre, acier, caoutchouc, etc.) pour les systmes de stockage et tuyauteries. Les bouchons des flacons de ractifs sont prvus avec un joint poreux spcial qui permet lchappement de gaz. Le bouchon dorigine doit toujours tre utilis sur le flacon deau oxygne. A titre de prcaution, les flacons de ractifs sont expdis dans un sac plastique. Sil existe des traces de fuites pendant le transport, porter des gants pour retirer le flacon du sac et rincer le flacon leau aprs lavoir sorti du sac. Rincer le sac avant limination.
3.8
Utilisation de lacide sulfurique

Lire et observer tous les avertissements sur les tiquettes des produits et la fiche de donnes de scurit du produit qui accompagne lacide sulfurique. Lacide sulfurique concentr utilis dans lopration de minralisation doit tre manipul correctement et avec prcaution. Lacide sulfurique est un acide fort et un oxydant puissant qui peut provoquer des brlures graves au contact de la peau et des lsions irrversibles sil est mis au contact des yeux. Cette action corrosive est beaucoup plus grave si lacide est chaud. En cas de contact avec les yeux ou la peau, laver les yeux et/ 19
ou la peau leau pendant 15 minutes. Retirer les vtements contamins. Appeler un mdecin. Lacide sulfurique sous forme de brouillard ou de vapeur a t class comme cancrigne possible pour lhomme par lAgence Internationale de Recherche sur le Cancer (IARC). Lacide sulfurique est un oxydant puissant. Il peut provoquer un feu ou exploser au contact de nombreux produits chimiques diffrents. Suivre les rgles de stockage appropries.
3.9
Nettoyage des dversements et fuites

Prendre les plus grandes prcautions pour nettoyer des fuites ou produits rpandus pendant toute la technique de digestion. Votre socit peut exiger que seules des personnes habilites portant les quipements de protection appropris (gants, lunettes de scurit, masques de protection et vtements rsistants aux agents chimiques) interviennent en cas de dversement ou de fuite. Un dversement, dbordement ou une projection par le minralisateur Digesdahl peut laisser un rsidu sur le matriel ou dautres surfaces. Le nettoyage du rsidu doit tre fait avec prcaution. Veuillez observer les mesures de scurit ci-dessous : 1. NE PAS tenter de nettoyer lappareil pendant quil est chaud, ceci peut causer la rupture du verre. Laisser refroidir lappareil avant de le nettoyer. 2. Dbrancher 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 leau pour la dcontaminer. 4. Essuyer les surfaces extrieures de lappareil Digesdahl (plaque chauffante, commandes lectriques, etc.) et autres surfaces du laboratoire plusieurs fois avec un tissu humide ou un papier dessuyage. 5. Ne pas rincer ou arroser lappareil directement, ceci pourrait le dtriorer. 6. Eliminer les papiers et tissus de faon approprie, ils peuvent avoir t contamins par lchantillon ou les rsidus chimiques.
20
SECTION 4
4.1
OPERATION
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.
Apparatus Preparation
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 vtements de protection. Un acide fort (acide sulfurique concentr) et un oxydant puissant (peroxyde d'hydrogne 50%) sont utiliss dans la raction de minralisation. Ces produits chimiques peuvent causer des brlures s'ils sont projets sur la peau ou des blessures irrversibles aux yeux s'ils sont mis au contact des yeux. Si ces produits sont chauds, les effets sont considrablement plus graves. Immdiatement rincer toute partie atteinte abondamment l'eau et consulter un mdecin.
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

Sample Type
Plant tissue Meat & Poultry Fluid Fertilizers
Sample Weight
0.25 to 0.5 g 0.5 g or predigestion 0.1 to 0.25 g
Vol. of Acid
4 mL 4 mL or as in predigest 4 mL
Preheat Time (Step 5)

4 min. 4 min. 4 min.
Vol. of Peroxide
10 mL 10 mL 10 mL
Special Instructions
Use Nitrogen-free paper to weigh samples. Add 0.4 g Kjeldahl Reduction 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. Use Nitrogen-free paper to weigh samples. Preheat acid for 1 minute then add sample through funnel. Heat flask for 30 seconds after sample is in the flask. Heat the diluted digest for 15 minutes and filter. Water must evaporate before acid will reflux. Boiling chips required. Water must evaporate before acid will reflux. Boiling chips required. Weigh samples into flake and record exact weight. Digest will be clear with particles on bottom if metal oxides are not 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. Heat the diluted digest for 15 min. and filter. Lower heater temperature if foaming or burning occurs.
Feed & Forage Dairy Cereal Beverage
0.25 g 0.25 to 2.0 g 0.25 to 0.5 g about 5 g (pipet into funnel
4 mL 4 mL 4 mL 4 mL
4 min. 4 min. 4 min. 1 min.
10 mL 10 mL 10 mL 10 mL
Sludge
<2.5 g wet sludge <0.5 g dried sludge not more than 0.5 g solid (mL = 40/C; C= % solids) 0.3 to 10 mL
4 mL
3-5 min.
10 mL of increase in 5 mL increments 10 mL or increase in 5 mL increments 10 mL
Water & Wastewater Bath Solutions Edible Oils
3 mL
until acid is refluxing 4 min.
4 mL
0.25 to 0.5 g
4-6 mL
4 min.
5 mL immediately and 5 mL later 20 mL
Ion Exchange Resins
equivalent of 0.25 g dry resin
10-15 mL
12 min.
Soil Fuels
0.25 to 0.5 g 0.25 to 0.5 g
6 mL 6 mL
4 min. 4 min.
10-20 mL 20 mL
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 + 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 Formula Structure C7H11O3SN Glycine PTSA C9H13O5SN Nicotinic Acid PTSA C13H13O5SN
Molecular Weight Melting Point, C % Nitrogen % Protein Digestability Index Moisture Absorption at 25 % RH at 50% RH at 90% RH
189.235 7.402 46.261 0
247.277 199 5.664 35.403 3
295.316 179 4.743 29.643 10
0.04% 0.07% 0.14%
0.03% 0.047% 0.15%
0.00% 0.01% 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 scurit avant deffectuer cette technique de digestion.
28
GENERAL DIGESDAHL DIGESTION
1. Transfer a preweighed or a premeasured amount of sample into a 100-mL Digesdahl digestion flask; see Table 1 on page 22. The amount transferred should not contain more than 0.5 g of solids or organic liquids. The maximum volume for water samples is 40 mL. In samples with more than 1% solids present, use the formula below:
Water Sample Volume = 40 % solids
2. Add concentrated sulfuric acid (according to Table 1 on page 22) to the volumetric flask and at least two silicon carbide boiling chips for liquid samples.
Note: Pretreat boiling chips by soaking in 1:1 Nitric Acid and rinsing thoroughly with deionized water. Treatment is very important in low-level work. Hach recommends silicon carbide boiling chips.
3. Turn on the water to the aspirator and make sure there is suction to the fractionating column. Turn the temperature dial to a heat setting of 440 C (825 F). For meat digestion, set to 468 C (875 F).
Note: Wait for the proper temperature to be reached before the sample is placed on the heater.
4. Place the flask weight followed by the fractionating column with funnel on the flask. Place the flask on the heater and heat until the sulfuric acid boils (refluxing sulfuric acid will be visible).
Note: White acid vapors usually will be present, but their presence alone does not indicate that the boiling point of sulfuric acid has been reached. Note: Liquid samples require total evaporation of water before vapors are visible. Note: If sample foams up into the neck of the flask, lower temperature to 335 C (635 F). Continue heating at lower temperature until all water is evaporated. Then return to original digestion temperature. Note: If foaming or bumping is not stopped by lowering temperature or volume, then liquid samples that will not clog the capillary funnel may be added to the flask via the capillary funnel, 10 mL at a time. Decrease amount added if foaming persists.
Note: Use only Hach digestion flasks. Volumetric flasks with concave bottoms should not be used. Note: If solids are 10% of total volume of sample, the maximum volume of liquid sample would be 4 mL. Note: Several 40-mL sample aliquots of the sample may be digested in succession to concentrate a sample. Note: If liquid is too viscous to measure, preweigh the sample into the digestion flask.
29
GENERAL DIGESDAHL DIGESTION, continued

3-5 minutes
5. Heat 3-5 minutes.

Do not boil sample to dryness. If sulfuric acid is not present after heating, do not proceed with Step 6. Discard the sample if it evaporates to dryness. Start over and use a larger volume of sulfuric acid in Step 2 of this procedure. Or chose a smaller sample amount for digestion.
Note: Some organic samples may need more than five minutes for complete digestion. See Table 1 on page 22.
6. Do not proceed if sulfuric acid is not visible in the flask. Add 10 mL of 50% Hydrogen Peroxide to the charred sample via the funnel on the fractionating head.
Note: Visually confirm the presence of sulfuric acid in the flask before adding hydrogen peroxide.
7. After addition of hydrogen peroxide is complete, boil off excess hydrogen peroxide by heating for one more minute. Do not heat to dryness.
8. Take the hot flask off the heater and allow the flask to cool. Remove the fractionating column from the digestion flask.
Note: Use finger cots to remove the digestion flask. Place it on a cooling pad for at least one minute. Then remove the column.
Note: If the sample goes to dryness, turn off the Digesdahl and air cool to room temperature. Add Note: If the digest does not water to flask before handling. Repeat the turn colorless, add digestion from the Step 1 5 mL increments of using a new sample. peroxide until the digest becomes clear. Note: Use long-neck glassware or a pipet to transfer the hydrogen peroxide.
30
Use metals or TKN procedure
9. Dilute the digest with 10. Turn the

approximately 70 mL of deionized water. If not analyzing for aluminum, nickel or iron, dilute to the 100-mL mark with deionized water; skip Step 10 and proceed to Step 11. If analyzing for nickel, aluminum or iron, go to Step 10. temperature dial to a heat setting of 204 C (400 F). Add 150 mL of water to a 400-mL beaker. Place the beaker on the heater. Place the flask in the beaker and boil for 15 minutes. Air cool to room temperature and dilute to the 100-mL mark with deionized water. Invert Note: Add deionized water slowly at first. Cool several times to mix.
the flask if necessary for handling.
11. If the sample has 12. Continue the visible turbidity, filter analysis using one of the or wait until the following procedures. turbidity settles, and the upper portion of the sample is clear.
Filter as follows: a) Place a filter paper into
the filter holder with wrinkled surface upward.
b) Place the filter holder

assembly in the filtering flask and wet the filter with deionized water to ensure adhesion to the holder.
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 coprecipitate 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). 4. Add one drop of 1 N KOH. Stopper the cylinder and invert several 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. 6. Add deionized water to the volume indicated in the colorimetric 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 premeasured amount of sample into a 100-mL Digesdahl digestion flask; see Sample and Analysis Volume Tables for Aqueous Liquids following this procedure. The amount transferred should not contain more than 0.5 g of material which is not water. The maximum volume for water samples is 40 mL. In samples with more than 1% solids present, use the formula below:
Water Sample Volume = 40 %solids
2. Add 3 mL of concentrated sulfuric acid (spec. gravity 1.84) to the volumetric flask and two or more silicon carbide (carborundum) boiling chips for liquid samples.
Note: Pretreat boiling chips by soaking in 1:1 Nitric Acid and rinsing thoroughly with deionized water. Treatment is very important in low-level work. Hach recommends using silicon carbide boiling chips.
3. Turn the temperature dial to a heat setting of 440 C (825 F). When the proper temperature is reached, turn on the water to the aspirator and make sure there is suction to the fractionating column.
Note: Wait for the proper temperature to be reached before sample is placed on the heater. Note: Always operate the Digesdahl apparatus with a safety shield in place or inside a closed fume hood. Safety glasses are mandatory.
4. Place the flask weight followed by the fractionating column with funnel on the flask. Place the flask on the heater and heat until the sulfuric acid boils (refluxing sulfuric acid will be visible).
Note: White acid vapors will usually be present but their presence alone does not indicate that the boiling point of sulfuric acid has been reached. Note: Aqueous samples require total evaporation of water before vapors are visible. Note: If sample foams up into the neck of the flask, lower temperature to 335 C (635 F). Continue heating at a lower temperature until all water is evaporated. Then return to original digestion temperature. Note: If foaming or bumping is not stopped by lowering temperature or volume, then liquid samples that will not clog the capillary funnel may be added to the flask via the capillary funnel, 10 mL at a time. Decrease amount added if foaming persists.
Note: Use only Hach Digesdahl flasks. Volumetric flasks with concave bottoms should not be used. Note: If solids are 10% of total volume of sample, the maximum volume of liquid sample would be 4 mL. Note: Oils and organics should be considered as solids when determining sample size. Note: If liquid is too viscous to measure, preweigh the sample into the digestion flask.
39
DIGESTION PROCEDURE FOR AQUEOUS LIQUIDS, continued

4:00
5. Boil 4 more minutes. 6. Do not proceed if

Do not boil the sample to dryness. If sulfuric acid is not present in the flask after the 4 minute heating, do not proceed with Step 6! Discard sample if it evaporates to dryness. Start over and use a larger volume of sulfuric acid in Step 2 of this procedure. Or choose a smaller sample amount for digestion. sulfuric acid is not visible in the flask! Add 10 mL of 50% Hydrogen Peroxide to the charred sample via the funnel on the fractionating column.
Note: Visually confirm the presence of sulfuric acid in the flask before adding hydrogen peroxide.
7. After addition of hydrogen peroxide is complete, boil off excess hydrogen peroxide by heating for one more minute. Do not heat to dryness.
8. Take the hot flask off the heater and allow the flask to cool. Remove the fractionating column from the digestion flask.
Note: Use finger cots to remove the digestion flask. Place it on a cooling pad for at least one minute. Then remove the column. Do not add water to the flask until it has cooled.
Note: If the sample goes to dryness, turn off the Digesdahl and air cool to room temperature. Add Note: If the digest does not water to flask before handling. Repeat the turn colorless, add 5 mL digestion from the increments of hydrogen beginning using a new peroxide until the digest 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 approximately 70 mL with deionized water.
10. If analyzing for aluminum, nickel or iron, continue to Step 11. Note: Add deionized water If analyzing for other substances, dilute to the slowly at first. Cool the 100-mL mark with flask if necessary for handling. deionized water; skip Step 11 and go to Step 12.
11. Turn the temperature dial to a heat setting of 204 C (400 F). Add 150 mL of water to a 400-mL beaker. Place the beaker on the heater. Place the flask in the beaker and boil for 15 minutes. Air cool to room temperature and dilute to the 100-mL mark with deionized water. Invert several times to mix.
12. If the sample has visible turbidity, filter or wait until the turbidity settles, and the upper portion of the sample is clear.
Filter as follows: a) Place a filter paper into

c) While applying a

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.
1. Pipet the appropriate analysis volume into the appropriate mixing graduate cylinder. See Sample and Analysis Volume Tables for Aqueous Liquids following this procedure to determine the analysis volume.
41

Note: High iron content will cause precipitation (brown cloud) which will coprecipitate 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. 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 8 N KOH Standard Solution, one drop at a time, swirling between each addition, until the first flash of pale blue appears (pH 3). 4. Add one drop of 1 N KOH. Stopper the cylinder and invert several times to mix.
5. Continue to add 1 N KOH in this manner until the first permanent blue color appears.
42

6. Add deionized water to the volume indicated in the colorimetric procedure. 7. Continue with 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 conc. (mg/L)
0.1-5 0.5-20 2.0-80 20-800 200-8000 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
Sample amount (mL)

40.0 20.0 10.0 5.00 1.00
Analysis Volume (mL)

20.0 10.0 5.00 1.00 0.50
Dilute to
50.0 mL 50.0 mL 50.0 mL 50.0 mL 50.0 mL
Aluminum, ECR (Method 8326) Expected Al conc. (mg/L)

0.05-1.3 0.2-5.5 0.8-22 8.0-220 80-2200 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
Sample amount (mL)

40.0 20.0 10.0 5.00 1.00

20.0 10.0 5.00 1.00 0.50
Dilute to
50.0 mL 50.0 mL 50.0 mL 50.0 mL 50.0 mL
43

Cadmium, Dithizone (Method 8017) Expected Cd conc. (g/L)
0.05-2.5 0.2-10 1-40 10-400 100-4000 A 25 = g/L Total Cd ----------------B C A = g/L reading from instrument B = mL sample amount from table C = mL analysis volume from table
Sample amount (mL)

40.0 20.0 10.0 5.00 1.00

20.0 10.0 5.00 1.00 0.50
Dilute to
250 mL 250 mL 250 mL 250 mL 250 mL
Chromium, Total (Method 8024) Expected Cr conc. (mg/L)

0.05-1.8 0.20-7.5 0.75-30 7.5-300 75-3000 A 2500 ----------------------- = mg/L Total Cr B C A = mg/L reading from instrument B = mL sample amount from table C = mL analysis volume from table
Sample amount (mL)

40.0 20.0 10.0 5.00 1.00

20.0 10.0 5.00 1.00 0.50
Dilute to
25.0 mL 25.0 mL 25.0 mL 25.0 mL 25.0 mL
44

Cobalt (Method 8078) Expected Co conc. (mg/L)
0.1-6.0 0.5-25 2.0-100 20-1000 200-10000 A 2500 ----------------------- = mg/L Total Co B C A = mg/L reading from instrument B = mL sample amount from table C = mL analysis volume from table
Sample amount (mL)

40.0 20.0 10.0 5.00 1.00

20.0 10.0 5.00 1.00 0.50
Dilute to
25.0 mL 25.0 mL 25.0 mL 25.0 mL 25.0 mL
Copper, Bicinchoninate (Methods 8026 and 8506) Expected Cu conc. (mg/L)

0.25-15 1-60 4-240 40-2400 400-24000 A 2500 ----------------------- = mg/L Total Cu B C A = mg/L reading from instrument B = mL sample amount from table C = mL analysis volume from table
Sample amount (mL)

40.0 20.0 10.0 5.00 1.00

20.0 10.0 5.00 1.00 0.50
Dilute to
25.0 mL 25.0 mL 25.0 mL 25.0 mL 25.0 mL
45

Iron, 1,10 Phenanthroline (Method 8008) Expected Fe conc. (mg/L)
0.15-8 0.6-35 2.5-125 25-1250 250-12500 A 2500 ----------------------- = mg/L Total Fe B C A = mg/L reading from instrument B = mL sample amount from table C = mL analysis volume from table
Sample amount (mL)

40.0 20.0 10.0 5.00 1.00

20.0 10.0 5.00 1.00 0.50
Dilute to
25.0 mL 25.0 mL 25.0 mL 25.0 mL 25.0 mL
Iron, Ferrozine (Method 8147) Expected Fe conc. (mg/L)

0.07-4 0.3-15 1.1-65 11-650 110-6500 A 2500 ----------------------- = mg/L Total Fe B C A = mg/L reading from instrument B = mL sample amount from table C = mL analysis volume from table
Sample amount (mL)

40.0 20.0 10.0 5.00 1.00

20.0 10.0 5.00 1.00 0.50
Dilute to
25.0 mL 25.0 mL 25.0 mL 25.0 mL 25.0 mL
46

Lead, Dithizone (Method 8033) Expected Pb conc. (g/L)
0.1-5.0 0.4-20 1.5-80 15-800 150-8000 A 25 = g/L Total Pb ----------------B C A = g/L reading from instrument B = mL sample amount from table C = mL analysis volume from table
Sample amount (mL)

40.0 20.0 10.0 5.00 1.00

20.0 10.0 5.00 1.00 0.50
Dilute to
250 mL 250 mL 250 mL 250 mL 250 mL
Manganese, PAN (Method 8149) Expected Mn conc. (mg/L)

0.05-2.1 0.2-8.7 0.8-35 8-350 80-3500 A 2500 ----------------------- = mg/L Total Mn B C A = mg/L reading from instrument B = mL sample amount from table C = mL analysis volume from table
Sample amount (mL)

40.0 20.0 10.0 5.00 1.00

20.0 10.0 5.00 1.00 0.50
Dilute to
25.0 mL 25.0 mL 25.0 mL 25.0 mL 25.0 mL
47

Nickel, PAN (Method 8150) Expected Ni conc. (mg/L)
0.05-3 0.2-12 0.8-47 8-470 80-4700 A 2500 ----------------------- = mg/L Total Ni B C A = mg/L reading from instrument B = mL sample amount from table C = mL analysis volume from table
Sample amount (mL)

40.0 20.0 10.0 5.00 1.00

20.0 10.0 5.00 1.00 0.50
Dilute to
25.0 mL 25.0 mL 25.0 mL 25.0 mL 25.0 mL
Nitrogen TKN (Method 8075) Expected Nitrogen conc. (mg/L)

0.5-28 2-112 11-560 45-2250 425-22500
Sample amount (mL)

40.0 20.0 10.0 5.00 1.00

10.0* 5.00* 2.00* 1.00* 0.50*
Dilute to
25.0 mL* 25.0 mL* 25.0 mL* 25.0 mL* 25.0 mL*
*These are guidelines only. See the spectrophotometer procedure manual. A 75 ----------------- = mg/L TKN B C A = mg/L reading from instrument B = mL sample amount from table C = mL analysis volume from table
48

Phosphorus, Ascorbic Acid (Method 8048) Expected PO4 conc. (mg/L)
0.12-6 0.5-23 2-90 20-900 200-9000
Sample amount (mL)

40.0 20.0 10.0 5.00 1.00

20.0 10.0 5.00 1.00 0.50
Dilute to
25.0 mL 25.0 mL 25.0 mL 25.0 mL 25.0 mL
A 2500 ----------------------- = mg/L Total PO4 B C A = mg/L reading from instrument B = mL sample amount from table C = mL analysis volume from table
Potassium (Method 8049) Expected K conc. (mg/L)

4-20 15-80 60-300 200-1000 600-3000 2000-10000 6000-30000 A 2500 ----------------------- = mg/L Total K B C A = mg/L reading from instrument B = mL sample amount from table C = mL analysis volume from table
Sample amount (mL)

40.0 20.0 10.0 5.0 5.00 3.0 1.00

20.0 10.0 5.00 3.00 1.00 0.500 0.50
Dilute to
25.0 mL 25.0 mL 25.0 mL 25.0 mL 25.0 mL 25.0 mL 25.0 mL
49

Silver (Method 8120) Expected Ag conc. (mg/L)
0.08-3.7 0.3-15 1.0-60 12-600 120-6000 A 5000 ----------------------- = mg/L Total Ag B C A = mg/L reading from instrument B = mL sample amount from table C = mL analysis volume from table
Sample amount (mL)

40.0 20.0 10.0 5.00 1.00

20.0 10.0 5.00 1.00 0.50
Dilute to
50.0 mL 50.0 mL 50.0 mL 50.0 mL 50.0 mL
Zinc (Method 8009) Expected Zn conc. (mg/L)

0.2-12.5 0.8-50 3.0-200 30-2000 300-20000 A 5000 ----------------------- = mg/L Total Zn B C A = mg/L reading from instrument B = mL sample amount from table C = mL analysis volume from table
Sample amount (mL)

40.0 20.0 10.0 5.00 1.00

20.0 10.0 5.00 1.00 0.50
Dilute to
50.0 mL 50.0 mL 50.0 mL 50.0 mL 50.0 mL
50
51
Danger
Danger
52
DIGESTION PROCEDURE FOR OILS
1. Transfer 0.25 g or less of sample into a 100-mL Digesdahl digestion flask; see Sample and Analysis Volume Tables for Oils following this procedure.
Note: Take care to ensure you have a homogenous sample.
2. Add 4 mL concentrated sulfuric acid (spec. gravity 1.84) to the digestion flask.
3. Turn the temperature dial to a heat setting of 440 C (825 F). When the proper temperature is reached, turn on the Note: Use only Hach Digesdahl digestion flasks. water to the aspirator and make sure there is Volumetric flasks with concave bottom should not suction to the be used. fractionating column.
4. Place the flask weight followed by the fractionating column with funnel on the flask. Place the flask on the heater and boil 4 minutes. Do not boil to dryness! If sulfuric acid is not present in the flask after the boiling Note: Safety glasses and Note: Wait for the proper 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.
Note: If sample foams up into the neck of the flask, 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
of 50% hydrogen peroxide to the charred sample via the funnel on the fractionating head.
Note: Visually confirm the presence of sulfuric acid in the flask before adding hydrogen peroxide. Note: If the digest does not turn colorless, add 5 mL increments of peroxide until the digest becomes clear or does not change color. Note: If sample foams 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.
6. After addition of
hydrogen peroxide by heating for one more minute. Do not heat to dryness.
7. Take the hot flask off 8. Dilute the digest

the fractionating column Note: Add demineralized from the digestion flask. water slowly at first. Cool
the flask if necessary for handling.
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.
Note: Use finger cots to remove the digestion flask. Note: If the sample goes to Place it on a cooling pad for at least one minute. dryness, turn off the Then remove the column. Digesdahl and air cool Do not add water to the completely. Add water flask until it has cooled. to flask before handling. Repeat digestion from the beginning using a new sample.
54
9. If analyzing for
aluminum, nickel or iron, continue to Step 10. If analyzing for other substances, dilute to the 100-mL mark with deionized water; Skip Step 10 and go to Step 11.
10. Turn the temperature dial to a heat setting of 204 C (400 F). Add 150 mL of water to a 400-mL beaker. Place the beaker on the heater. Place the flask in the beaker and boil for15 minutes. Cool to room temperature and dilute to the mark with demineralized water. Invert several times to mix.
Note: When using a Digesdahl Digestion Apparatus system without temperature control dials, reset to a lower setting that gently boils the water.
11. If the sample is visibly turbidity, filter or wait until the turbidity settles, and the upper portion of the sample is clear.
Filter as follows:
12. Continue the analysis using the appropriate procedure below.
a) Place a filter paper into


assembly in the filtering flask and wet the filter with demineralized water to ensure adhesion to the holder.
c) While applying a

Metals Method
1. Pipet the appropriate analysis volume into the appropriate mixing graduate cylinder. See Sample and Analysis Volume Tables for Oils following the specific digestion to determine the analysis volume.
Note: Some methods require pipetting into a volumetric flask or a regular graduated cylinder.
2. Dilute to about 20 mL with deionized water. 55

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: High iron content will cause precipitation (brown cloud) which will co-precipitate other metals. Repeat this procedure with a smaller aliquot volume.
56

Sample and Analysis Volume Tables for Oils

Aluminum, Aluminon (Method 8012) Expected Al conc. (mg/kg)
15-800 40-2000 100-5300 1000-40000 A 5000 ----------------------- = mg/kg Total Al B C A = mg/L reading from instrument B = g sample amount from table C = mL analysis volume from table
Sample amount (g)

0.250 0.200 0.150 0.100

20.0 10.0 5.00 1.00
Aluminum, ECR (Method 8326) Expected Al conc. (mg/kg)

7-220 20-550 50-1400 400-11000 A 5000 ----------------------- = mg/kg Total Al B C A = mg/L reading from instrument B = g sample amount from table C = mL analysis volume from table
Sample amount (g)

0.250 0.200 0.150 0.100

20.0 10.0 5.00 1.00
57

Cadmium, Dithizone (Method 8017) Expected Cd conc. (mg/kg)
10-400 25-1000 65-2600 480-20000 A 25 ----------------- = mg/kg Total Cd B C A = g/l reading from instrument B = g sample amount from table C = mL analysis volume from table
Sample amount (g)

0.250 0.200 0.150 0.100

20.0 10.0 5.00 1.00
Chromium, Total (Method 8024) Expected Cr conc. (mg/kg)

8-300 20-750 50-2000 350-15000 A 2500 ----------------------- = mg/kg Total Cr B C A = mg/L reading from instrument B = g sample amount from table C = mL analysis volume from table
Sample amount (g)

0.250 0.200 0.150 0.100

20.0 10.0 5.00 1.00
58

Cobalt (Method 8078) Expected Co conc. (mg/kg)
15-950 45-2400 120-6200 880-46000 A 2500 ----------------------- = mg/kg Total Co B C A = mg/L reading from instrument B = g sample amount from table C = mL analysis volume from table
Sample amount (g)

0.250 0.200 0.150 0.100

20.0 10.0 5.00 1.00
Copper, Bicinchoninate (Methods 8026 and 8506) Expected Cu conc. (mg/kg)

40-2300 100-6000 320-15000 2000-110000 A 2500 ----------------------- = mg/kg Total Cu B C A = mg/L reading from instrument B = g sample amount from table C = mL analysis volume from table
Sample amount (g)

0.250 0.200 0.150 0.100

20.0 10.0 5.00 1.00
59

Iron, 1,10 Phenanthroline (Method 8008) Expected Fe conc. (mg/kg)
25-1400 60-3500 160-9300 1200-70000 A 2500 ----------------------- = mg/kg Total Fe B C A = mg/L reading from instrument B = g sample amount from table C = mL analysis volume from table
Sample amount (g)

0.250 0.200 0.150 0.100

20.0 10.0 5.00 1.00
Iron, Ferrozine (Method 8147) Expected Fe conc. (mg/kg)

11-650 30-1600 75-4300 560-32000 A 2500 ----------------------- = mg/kg Total Fe B C A = mg/L reading from instrument B = g sample amount from table C = mL analysis volume from table
Sample amount (g)

0.250 0.200 0.150 0.100

20.0 10.0 5.00 1.00
60

Lead, Dithizone (Method 8033) Expected Pb conc. (mg/kg)
15-800 38-2000 100-5300 750-40000 A 25 ----------------- = mg/kg Total Pb B C A = g/l reading from instrument B = g sample amount from table C = mL analysis volume from table
Sample amount (g)

0.250 0.200 0.150 0.100

20.0 10.0 5.00 1.00
Manganese, PAN (Method 8149) Expected Mn conc. (mg/kg)

7-350 20-870 50-2300 400-17000 A 2500 ----------------------- = mg/kg Total Mn B C A = mg/L reading from instrument B = g sample amount from table C = mL analysis volume from table
Sample amount (g)

0.250 0.200 0.150 0.100

20.0 10.0 5.00 1.00
61

Nickel, PAN (Method 8150) Expected Ni conc. (mg/kg)
7-470 20-1200 50-3100 350-23000 A 2500 ----------------------- = mg/kg Total Ni B C A = mg/L reading from instrument B = g sample amount from table C = mL analysis volume from table
Sample amount (g)

0.250 0.200 0.150 0.100

20.0 10.0 5.00 1.00
Nitrogen TKN (Method 8075) Expected Nitrogen conc. (mg/kg)

85-4500 210-11000 2100-110000
Sample amount (g)

0.250 0.200 0.100

10.0* 5.00* 1.00*
*These are guidelines only. See the spectrophotometer procedure manual. A 75 ----------------- = mg/kg TKN B C A = mg/L reading from instrument B = g sample amount from table C = mL analysis volume from table
62

Phosphorus, Ascorbic Acid (Method 8048) Expected PO4 conc. (mg/kg)
20-900 50-2300 130-6200 1000-45000 A 2500 ----------------------- = mg/kg Total PO4 B C A = mg/L reading from instrument B = g sample amount from table C = mL analysis volume from table
Sample amount (g)

0.250 0.200 0.150 0.100

20.0 10.0 5.00 1.00
Potassium (Method 8049) Expected K conc. (mg/kg)

600-3400 1500-8500 4100-22000 15500-85000 31000-170000 A 2500 ----------------------- = mg/kg Total K B C A = mg/L reading from instrument B = g sample amount from table C = mL analysis volume from table
Sample amount (g)

0.250 0.200 0.150 0.100 0.100

20.0 10.0 5.00 2.00 1.00
63

Silver (Method 8120) Expected Ag conc. (mg/kg)
12-600 30-1500 80-4000 620-30000 A 5000 ----------------------- = mg/kg Total Ag B C A = mg/L reading from instrument B = g sample amount from table C = mL analysis volume from table
Sample amount (g)

0.250 0.200 0.150 0.100

20.0 10.0 5.00 1.00
Zinc (Method 8009) Expected Zn conc. (mg/kg)

30-2000 80-5000 200-13000 1600-100000 A 5000 ----------------------- = mg/kg Total Zn B C A = mg/L reading from instrument B = g sample amount from table C = mL analysis volume from table
Sample amount (g)

0.250 0.200 0.150 0.100

20.0 10.0 5.00 1.00
64
65
Danger
Danger
66
DIGESTION PROCEDURE FOR SOLIDS
1. Transfer 0.50 g or less of sample into a 100-mL Digesdahl digestion flask; see Sample and Analysis Volume Tables for Solids following this procedure.
4. Place the flask weight followed by the fractionating column with funnel on the flask. Place the flask on the heater and boil 4 minutes. Do not boil to dryness! If sulfuric acid is not present in the Note: Be sure you have a flask after the boiling Note: Safety glasses and a Note: Wait for the proper homogenous sample. Solid safety shield placed period, do not proceed temperature to be reached sample should be finely between the operator and before sample is placed on to Step 5! Discard the ground or chopped and the Digesdahl are required. the heater. sample and use more mixed well. sulfuric acid for the digestion procedure in Step 2. Or choose a smaller amount from the Sample and Analysis Volume Tables for Solids.
Note: If sample foams up into the neck of the flask, 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.
2. Add 4 mL concentrated sulfuric acid (spec. gravity 1.84) to the digestion flask.
3. Turn the temperature dial to a heat setting of 440 C (825 F). When the proper temperature is reached, turn on the Note: Use only Hach Digesdahl digestion flasks. water to the aspirator and make sure there is Volumetric flasks with concave bottom should not suction to the be used. fractionating column.
67
DIGESTION PROCEDURE FOR SOLIDS, continued
5. Do not proceed if
sulfuric acid is not visible in the flask. Add 10 mL of 50% hydrogen peroxide to the charred sample via the funnel on the fractionating column.
6. After addition of hydrogen peroxide is complete, boil off excess hydrogen peroxide by heating for one more minute . Do not heat to dryness.
7. Take the hot flask off the heater and allow the flask to air cool. Remove the fractionating column from the digestion flask.
Note: Use finger cots to remove the digestion flask. Place it on a cooling pad for at least one minute. Then remove the column. Do not add water to the flask until it has cooled.
8. Dilute the digest to approximately 70 mL with deionized water.

Note: Add deionized water slowly at first. Cool the flask if necessary for handling.
Note: If the sample goes to Note: Do not heat to dryness. dryness, turn off the Note: Visually confirm the Digesdahl and air cool to presence of sulfuric acid in room temperature. Add water to flask before the flask before adding handling. Repeat the 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. Note: If sample foams 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 aluminum, nickel or iron, continue to Step 10. If analyzing for other substances, dilute to the 100-mL mark with deionized water; skip Step 10 and go to Step 11.
10. Turn the temperature dial to a heat setting of 204 C (400 F). Add 150 mL of water to a 400-mL beaker. Place the beaker on the heater. Place the flask in the beaker and boil for 15 minutes. Air cool to room temperature and dilute to the mark with deionized water. Invert several times to mix.
11. If the sample has visible turbidity, filter or wait until the turbidity settles, and the upper portion of the sample is clear.
Filter as follows:
12. Continue with the analysis using the appropriate procedure below.
a) Place a filter paper into


Note: When using a Digesdahl Digestion Apparatus system without temperature control dials, reset to a lower setting that c) While applying a vacuum to the filtering gently boils the water. flask, transfer the sample to the filtering apparatus.

vacuum from the filtering flask and transfer to another container. Note: If small aliquots (1.0 mL) are analyzed, filtration is not needed.
Metals Method
1. Pipet the appropriate analysis volume into the appropriate mixing graduate cylinder. See Sample and Analysis Volume Tables for Solids following the specific digestion to determine the analysis volume.
69

Note: High iron content will cause precipitation (brown cloud) which will co-precipitate other metals. Repeat this procedure with a smaller aliquot volume.
70

Sample and Analysis Volume Tables for Solids

Aluminum, Aluminon (Method 8012) Expected Al conc. (mg/kg)
10-400 25-1000 65-2600 480-20000 1900-80000 A 5000 ----------------------- = mg/kg Total Al B C A = mg/L reading from instrument B = g sample amount from table C = mL analysis volume from table
Sample amount (g)

0.500 0.400 0.300 0.200 0.100

20.0 10.0 5.00 1.00 0.50
Aluminum, ECR (Method 8326) Expected Al conc. (mg/kg)

4-100 10-270 25-730 180-5500 750-22000 A 5000 ----------------------- = mg/kg Total Al B C A = mg/L reading from instrument B = g sample amount from table C = mL analysis volume from table
Sample amount (g)

0.500 0.400 0.300 0.200 0.100

20.0 10.0 5.00 1.00 0.50
71

Cadmium, Dithizone (Method 8017) Expected Cd conc. (mg/kg)
5-200 12-500 30-1300 240-10000 960-40000 A 25 = mg/kg Total Cd ----------------B C A = g/l reading from instrument B = g sample amount from table C = mL analysis volume from table
Sample amount (g)

0.500 0.400 0.300 0.200 0.100

20.0 10.0 5.00 1.00 0.50
Chromium, Total (method 8024) Expected Cr conc. (mg/kg)

4.9-150 10-370 25-1000 190-7500 750-30000 A 2500 ----------------------- = mg/kg Total Cr B C A = mg/L reading from instrument B = g sample amount from table C = mL analysis volume from table
Sample amount (g)

0.500 0.400 0.300 0.200 0.100

20.0 10.0 5.00 1.00 0.50
72

Cobalt (Method 8078) Expected Co conc. (mg/kg)
10-450 20-1200 50-3000 500-20000 2000-100000 A 2500 ----------------------- = mg/kg Total Co B C A = mg/L reading from instrument B = g sample amount from table C = mL analysis volume from table
Sample amount (g)

0.500 0.400 0.300 0.200 0.100

20.0 10.0 5.00 1.00 0.50
Copper, Bicinchoninate (Methods 8026 and 8506) Expected Cu conc. (mg/kg)

20-1200 50-3000 120-7500 1000-60000 4000-240000 A 2500 ----------------------- = mg/kg Total Cu B C A = mg/L reading from instrument B = g sample amount from table C = mL analysis volume from table
Sample amount (g)

0.500 0.400 0.300 0.200 0.100

20.0 10.0 5.00 1.00 0.50
73

Iron, 1,10 Phenanthroline (Method 8008) Expected Fe conc. (mg/kg)
12-700 35-1700 85-4500 650-35000 2500-140000 A 2500 ----------------------- = mg/kg Total Fe B C A = mg/L reading from instrument B = g sample amount from table C = mL analysis volume from table
Sample amount (g)

0.500 0.400 0.300 0.200 0.100

20.0 10.0 5.00 1.00 0.50
Iron, Ferrozine (Method 8147) Expected Fe conc. (mg/kg)

6-300 15-800 40-2000 300-15000 1200-65000 A 2500 ----------------------- = mg/kg Total Fe B C A = mg/L reading from instrument B = g sample amount from table C = mL analysis volume from table
Sample amount (g)

0.500 0.400 0.300 0.200 0.100

20.0 10.0 5.00 1.00 0.50
74

Lead, Dithizone (Method 8033) Expected Pb conc. (mg/kg)
8-400 20-1000 50-2600 400-20000 1500-80000 A 25 = mg/kg Total Pb ----------------B C A = g/l reading from instrument B = g sample amount from table C = mL analysis volume from table
Sample amount (g)

0.500 0.400 0.300 0.200 0.100

20.0 10.0 5.00 1.00 0.50
Manganese, PAN (Method 8149) Expected Mn conc. (mg/kg)

4-170 10-430 25-1100 200-8700 750-35000 A 2500 ----------------------- = mg/kg total Mn B C A = mg/L reading from instrument B = g sample amount from table C = mL analysis volume from table
Sample amount (g)

0.500 0.400 0.300 0.200 0.100

20.0 10.0 5.00 1.00 0.50
75

Nickel, PAN (Method 8150) Expected Ni conc. (mg/kg)
4-220 10-580 25-1500 200-11000 750-45000 A 2500 ----------------------- = mg/kg Total Ni B C A = mg/L reading from instrument B = g sample amount from table C = mL analysis volume from table
Sample amount (g)

0.500 0.400 0.300 0.200 0.100

20.0 10.0 5.00 1.00 0.50
Nitrogen TKN (Method 8075) Expected Nitrogen conc. (mg/kg)

42-2200 106-5600 350-18000 1000-56000 4200-220000
Sample amount (g)

0.500* 0.400* 0.300* 0.200* 0.100*

10.0* 5.00* 2.00* 1.00* 0.50*
*These are guidelines only. See the spectrophotometer procedure manual. A 75 ----------------- = mg/kg TKN B C A = mg/L reading from instrument B = g sample amount from table C = mL analysis volume from table
76

Phosphorus, Ascorbic Acid (Method 8048) Expected PO4 conc. (mg/kg)
10-450 25-1100 67-3100 500-23000 2000-93000 A 2500 ----------------------- = mg/kg Total PO4 B C A = mg/L reading from instrument B = g sample amount from table C = mL analysis volume from table
Sample amount (g)

0.500 0.400 0.300 0.200 0.100

20.0 10.0 5.00 1.00 0.50
Potassium (Method 8049) Expected K conc. (mg/kg)

300-1700 800-4200 2000-11000 15000-85000 62000-300000 A 2500 ----------------------- = mg/kg Total K B C A = mg/L reading from instrument B = g sample amount from table C = mL analysis volume from table
Sample amount (g)

0.500 0.400 0.300 0.200 0.100

20.0 10.0 5.00 1.00 0.50
77

Silver (Method 8120) Expected Ag conc. (mg/kg)
6-300 15-750 40-2000 300-15000 1200-60000 A 5000 ----------------------- = mg/kg Total Ag B C A = mg/L reading from instrument B = g sample amount from table C = mL analysis volume from table
Sample amount (g)

0.500 0.400 0.300 0.200 0.100

20.0 10.0 5.0 1.00 0.50
Zinc (Method 8009) Expected Zn conc. (mg/kg)

16-1000 40-2500 100-6600 800-50000 3000-200000 A 5000 ----------------------- mg/kg Total Zn B C A = mg/L reading from instrument B = g sample amount from table C = mL analysis volume from table
Sample amount (g)

0.500 0.400 0.300 0.200 0.100

20.0 10.0 5.00 1.00 0.50
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
5.1
MAINTENANCE
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.
Fuse Replacement
5.2
Kit Replacement Parts

Unit Cat. No.
Description
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
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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.
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84
REPLACEMENT PARTS
REQUIRED REAGENTS
Description Quantity Required 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
Description Unit Cat. No.
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 Soln, 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 sension1 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
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HOW TO ORDER
87
REPAIR SERVICE
88
WARRANTY
89

Digesdahl® Digestion Apparatus Models 23130-20, Manual

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Digesdahl® Digestion Apparatus Models 23130-20, Manual

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23130-18

Digesdahl Digestion Apparatus

hm/ct 2/97 8 ed aa/dk Rev. 2, 9/99

TRADEMARKS OF HACH COMPANY

TABLE OF CONTENTS, continued

Use of Danger Messages, Cautions and Notes

Figure 1 Digesdahl Digestion Apparatus

CAPILLARY FUNNEL VENT TRAP CAP CAPILLARY FUNNEL ADAPTOR

VENT TRAP BODY

COLLUMN BAFFLE FRACTIONATING COLUMN

COLUMN RECEPTACLE SAFETY SHIELD

FLASK WEIGHT DIGESTION FLASK

POWER SWITCH MODE SWITCH

PREPARATION FOR USE

2.2.1 Heater Assembly Assemble the heater assembly as shown in Figure 2.

Figure 2 Heater Assembly

Figure 3 Fractionating Column and Exhaust Assembly

Selecting a Temperature Setting

SAFETY & ENVIRONMENTAL CONSIDERATIONS

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

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

For respiratory protection, use a fume hood or Hachs 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

Using Hydrogen Peroxide

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%.

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

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

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 wash eyes with plenty of water if contaminated and get medical

Do not use unapproved materials (brass, copper, carbon steel, rubber,

Using Sulfuric Acid

Clean Up of Spills and Leaks

CONSIDERATIONS DE SECURITE ET DENVIRONNEMENT

Poids dchantillon : Ne jamais minraliser un chantillon qui contient

Les huiles et liquides organiques doivent tre considrs comme des

Type dacide : Utiliser seulement lacide spcifi dans les techniques

Prendre soin de maintenir en place la chemine et le manchon de

Toujours effectuer les minralisations derrire un cran de protection

Pour une protection respiratoire, utiliser une hotte ou lpurateur de

NE PAS ajouter dalcool, dactone ou autre solvant organique dans la

Pendant la digestion, utiliser le rglage de temprature et le temps de

Lors de la minralisation dune nouvelle substance pour la premire

Porter une blouse ou un tablier de laboratoire pour protger la peau et

Porter des chaussures appropries pour protger les pieds des

Ne pas utiliser de verrerie ou appareils endommags. Eliminer et

Laisser le Digesdahl refroidir naturellement (dans lair ambiant). Leau

Utilisation de leau oxygne

NE PAS mlanger leau oxygne avec dautres ractifs sauf

NE PAS ajouter deau oxygne directement dans la colonne de

Leau oxygne doit tre ajoute la matire organique carbonise

NE PAS utiliser deau oxygne des concentrations suprieures

Cest un agent fortement oxydant. La nature chimique de leau

Il peut se dcomposer avec dgagement de chaleur et doxygne. La