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69

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 Solids
following the specific digestion to determine the analysis volume.

Note: Some methods require pipetting into a volumetric flask or a regular
graduate cylinder.

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.

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 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

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.

Note: If small aliquots
(

≤

1.0 mL) are analyzed,

filtration is not needed.

12.

Continue with the

analysis using the
appropriate procedure
below.

DIGESTION PROCEDURE FOR SOLIDS,

continued

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Содержание Digesdahl 23130-20

Страница 1: ...400 688 9809 www mamots com 0431 85178766...

Страница 2: ...sdahl 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 99 400 688 9809 www mamots com 0...

Страница 3: ...ol Just Add Water LeadTrak m ColiBlue24 ManVer MolyVer Mug O Meter NetSketcher NitraVer NitriVer NTrak OASIS On Site Analysis Results You Can TrustSM OptiQuant OriFlow OxyVer PathoScreen PbEx PermaChe...

Страница 4: ...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 11 199...

Страница 5: ...ed 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 th...

Страница 6: ...e 12 3 3 Using Sulfuric Acid 14 3 4 Clean Up of Spills and Leaks 14 3 5 Waste Management 15 CONSIDERATIONS DE SECURITE ET D ENVIRONNEMENT 16 3 6 Min ralisateur Digesdahl 16 3 7 Utilisation de l eau ox...

Страница 7: ...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 Repla...

Страница 8: ...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 ma...

Страница 9: ...ially 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...

Страница 10: ...ar with all safety procedures before handling any chemicals DANGER La manipulation des chantillons chimiques talons et r actifs peut tre dangereuse Lire les fiches de donn es de s curit des produits n...

Страница 11: ...2 400 688 9809 www mamots com 0431 85178766...

Страница 12: ...d 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...

Страница 13: ...SEMBLY CAPILLARY FUNNEL ADAPTOR POWER SWITCH TEMPERATURE CONTROL DIGESTION FLASK FLASK WEIGHT SAFETY SHIELD COLLUMN BAFFLE VENT TRAP BODY FRACTIONATING COLUMN COLUMN RECEPTACLE VERTICAL SUPPORT HEAT S...

Страница 14: ...ing 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 B...

Страница 15: ...6 2 2 Assembly 2 2 1 Heater Assembly Assemble the heater assembly as shown in Figure 2 Figure 2 Heater Assembly 400 688 9809 www mamots com 0431 85178766...

Страница 16: ...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 diges...

Страница 17: ...8 Figure 3 Fractionating Column and Exhaust Assembly 400 688 9809 www mamots com 0431 85178766...

Страница 18: ...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 ind...

Страница 19: ...10 400 688 9809 www mamots com 0431 85178766...

Страница 20: ...er 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...

Страница 21: ...drogen 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 slo...

Страница 22: ...ht 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 shipp...

Страница 23: ...th 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 aci...

Страница 24: ...l 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 re...

Страница 25: ...ordre des op rations indiqu Si la fiole va sec la retirer imm diatement du syst me de chauffage et la laisser refroidir la temp rature ambiante Ne jamais ajouter d eau oxyg n e une fiole d chantillon...

Страница 26: ...s endommag s Eliminer et remplacer tous les quipements endommag s Laisser le Digesdahl refroidir naturellement dans l air ambiant L eau froide peut briser le verre chaud 3 7 Utilisation de l eau oxyg...

Страница 27: ...aux concentrations auxquelles il est utilis dans l industrie et peut provoquer une combustion spontan e au contact imm diat ou prolong des combustibles Il peut se d composer avec d gagement de chaleur...

Страница 28: ...e r actifs sont pr vus avec un joint poreux sp cial qui permet l chappement de gaz Le bouchon d origine doit toujours tre utilis sur le flacon d eau oxyg n e A titre de pr caution les flacons de r act...

Страница 29: ...te Un d versement d bordement ou une projection par le min ralisateur Digesdahl peut laisser un r sidu sur le mat riel ou d autres surfaces Le nettoyage du r sidu doit tre fait avec pr caution Veuille...

Страница 30: ...dant 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 eff...

Страница 31: ...re 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...

Страница 32: ...dge 0 5 g dried sludge 4 mL 3 5 min 10 mL of increase in 5 mL increments Heat the diluted digest for 15 minutes and filter Water Wastewater not more than 0 5 g solid mL 40 C C solids 3 mL until acid i...

Страница 33: ...SO4 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 m...

Страница 34: ...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 a...

Страница 35: ...n 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 d...

Страница 36: ...27 DIGESTION PROCEDURES 400 688 9809 www mamots com 0431 85178766...

Страница 37: ...important safety information before performing this digestion procedure Danger Lire au chapitre 3 les informations importantes pour la s curit avant d effectuer cette technique de digestion 400 688 98...

Страница 38: ...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...

Страница 39: ...n peroxide Note If the digest does not turn colorless add 5 mL increments of peroxide until the digest becomes clear Note Use long neck glassware or a pipet to transfer the hydrogen peroxide 7 After a...

Страница 40: ...100 mL 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 fo...

Страница 41: ...se 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 p...

Страница 42: ...l 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 cy...

Страница 43: ...34 400 688 9809 www mamots com 0431 85178766...

Страница 44: ...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 sam...

Страница 45: ...36 SAMPLE TYPE AND SIZE continued Chart 2 For Oils 400 688 9809 www mamots com 0431 85178766...

Страница 46: ...37 High levels of iron may interfere with analysis of some parameters Chart 3 For Solids SAMPLE TYPE AND SIZE continued 400 688 9809 www mamots com 0431 85178766...

Страница 47: ...important safety information before performing this digestion procedure Danger Lire au chapitre 3 les informations importantes pour la s curit avant d effectuer cette technique de digestion 400 688 98...

Страница 48: ...e 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 fractionati...

Страница 49: ...oxide 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 hy...

Страница 50: ...t 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...

Страница 51: ...zed 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...

Страница 52: ...mg L reading from instrument B mL sample amount from table C mL analysis volume from table Expected Al conc mg L Sample amount mL Analysis Volume mL Dilute to 0 1 5 40 0 20 0 50 0 mL 0 5 20 20 0 10 0...

Страница 53: ...lysis Volume mL Dilute to 0 05 2 5 40 0 20 0 250 mL 0 2 10 20 0 10 0 250 mL 1 40 10 0 5 00 250 mL 10 400 5 00 1 00 250 mL 100 4000 1 00 0 50 250 mL Expected Cr conc mg L Sample amount mL Analysis Volu...

Страница 54: ...lysis Volume mL Dilute to 0 1 6 0 40 0 20 0 25 0 mL 0 5 25 20 0 10 0 25 0 mL 2 0 100 10 0 5 00 25 0 mL 20 1000 5 00 1 00 25 0 mL 200 10000 1 00 0 50 25 0 mL Expected Cu conc mg L Sample amount mL Anal...

Страница 55: ...alysis Volume mL Dilute to 0 15 8 40 0 20 0 25 0 mL 0 6 35 20 0 10 0 25 0 mL 2 5 125 10 0 5 00 25 0 mL 25 1250 5 00 1 00 25 0 mL 250 12500 1 00 0 50 25 0 mL Expected Fe conc mg L Sample amount mL Anal...

Страница 56: ...ysis Volume mL Dilute to 0 1 5 0 40 0 20 0 250 mL 0 4 20 20 0 10 0 250 mL 1 5 80 10 0 5 00 250 mL 15 800 5 00 1 00 250 mL 150 8000 1 00 0 50 250 mL Expected Mn conc mg L Sample amount mL Analysis Volu...

Страница 57: ...conc mg L Sample amount mL Analysis Volume mL Dilute to 0 05 3 40 0 20 0 25 0 mL 0 2 12 20 0 10 0 25 0 mL 0 8 47 10 0 5 00 25 0 mL 8 470 5 00 1 00 25 0 mL 80 4700 1 00 0 50 25 0 mL Expected Nitrogen c...

Страница 58: ...0 12 6 40 0 20 0 25 0 mL 0 5 23 20 0 10 0 25 0 mL 2 90 10 0 5 00 25 0 mL 20 900 5 00 1 00 25 0 mL 200 9000 1 00 0 50 25 0 mL Expected K conc mg L Sample amount mL Analysis Volume mL Dilute to 4 20 40...

Страница 59: ...Dilute to 0 08 3 7 40 0 20 0 50 0 mL 0 3 15 20 0 10 0 50 0 mL 1 0 60 10 0 5 00 50 0 mL 12 600 5 00 1 00 50 0 mL 120 6000 1 00 0 50 50 0 mL Expected Zn conc mg L Sample amount mL Analysis Volume mL Di...

Страница 60: ...51 400 688 9809 www mamots com 0431 85178766...

Страница 61: ...important safety information before performing this digestion procedure Danger Lire au chapitre 3 les informations importantes pour la s curit avant d effectuer cette technique de digestion 400 688 98...

Страница 62: ...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 4 Place the flask weight followed by the fractionat...

Страница 63: ...emaining peroxide 6 After addition of hydrogen peroxide is complete boil off excess hydrogen peroxide by heating for one more minute Do not heat to dryness Note If the sample goes to dryness turn off...

Страница 64: ...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 te...

Страница 65: ...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 proc...

Страница 66: ...e C mL analysis volume from table Aluminum ECR Method 8326 A mg L reading from instrument B g sample amount from table C mL analysis volume from table Expected Al conc mg kg Sample amount g Analysis V...

Страница 67: ...sis volume from table Expected Cd conc mg kg Sample amount g Analysis Volume mL 10 400 0 250 20 0 25 1000 0 200 10 0 65 2600 0 150 5 00 480 20000 0 100 1 00 Expected Cr conc mg kg Sample amount g Anal...

Страница 68: ...s volume from table Expected Co conc mg kg Sample amount g Analysis Volume mL 15 950 0 250 20 0 45 2400 0 200 10 0 120 6200 0 150 5 00 880 46000 0 100 1 00 Expected Cu conc mg kg Sample amount g Analy...

Страница 69: ...ysis volume from table Expected Fe conc mg kg Sample amount g Analysis Volume mL 25 1400 0 250 20 0 60 3500 0 200 10 0 160 9300 0 150 5 00 1200 70000 0 100 1 00 Expected Fe conc mg kg Sample amount g...

Страница 70: ...s volume from table Expected Pb conc mg kg Sample amount g Analysis Volume mL 15 800 0 250 20 0 38 2000 0 200 10 0 100 5300 0 150 5 00 750 40000 0 100 1 00 Expected Mn conc mg kg Sample amount g Analy...

Страница 71: ...g sample amount from table C mL analysis volume from table Expected Ni conc mg kg Sample amount g Analysis Volume mL 7 470 0 250 20 0 20 1200 0 200 10 0 50 3100 0 150 5 00 350 23000 0 100 1 00 Expecte...

Страница 72: ...ble Expected PO4 conc mg kg Sample amount g Analysis Volume mL 20 900 0 250 20 0 50 2300 0 200 10 0 130 6200 0 150 5 00 1000 45000 0 100 1 00 Expected K conc mg kg Sample amount g Analysis Volume mL 6...

Страница 73: ...m table Expected Ag conc mg kg Sample amount g Analysis Volume mL 12 600 0 250 20 0 30 1500 0 200 10 0 80 4000 0 150 5 00 620 30000 0 100 1 00 Expected Zn conc mg kg Sample amount g Analysis Volume mL...

Страница 74: ...65 400 688 9809 www mamots com 0431 85178766...

Страница 75: ...important safety information before performing this digestion procedure Danger Lire au chapitre 3 les informations importantes pour la s curit avant d effectuer cette technique de digestion 400 688 98...

Страница 76: ...fractionating column Note Wait for the proper temperature to be reached before sample is placed on the heater 4 Place the flask weight followed by the fractionating column with funnel on the flask Pla...

Страница 77: ...with the remaining peroxide 6 After addition of hydrogen peroxide is complete boil off excess hydrogen peroxide by heating for one more minute Do not heat to dryness Note If the sample goes to dryness...

Страница 78: ...ture and dilute to the mark with deionized water Invert several times to mix Note When using a Digesdahl Digestion Apparatus system without temperature control dials reset to a lower setting that gent...

Страница 79: ...ionized 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...

Страница 80: ...ume from table Aluminum ECR Method 8326 A mg L reading from instrument B g sample amount from table C mL analysis volume from table Expected Al conc mg kg Sample amount g Analysis Volume mL 10 400 0 5...

Страница 81: ...Expected Cd conc mg kg Sample amount g Analysis Volume mL 5 200 0 500 20 0 12 500 0 400 10 0 30 1300 0 300 5 00 240 10000 0 200 1 00 960 40000 0 100 0 50 Expected Cr conc mg kg Sample amount g Analys...

Страница 82: ...pected Co conc mg kg Sample amount g Analysis Volume mL 10 450 0 500 20 0 20 1200 0 400 10 0 50 3000 0 300 5 00 500 20000 0 200 1 00 2000 100000 0 100 0 50 Expected Cu conc mg kg Sample amount g Analy...

Страница 83: ...e Expected Fe conc mg kg Sample amount g Analysis Volume mL 12 700 0 500 20 0 35 1700 0 400 10 0 85 4500 0 300 5 00 650 35000 0 200 1 00 2500 140000 0 100 0 50 Expected Fe conc mg kg Sample amount g A...

Страница 84: ...xpected Pb conc mg kg Sample amount g Analysis Volume mL 8 400 0 500 20 0 20 1000 0 400 10 0 50 2600 0 300 5 00 400 20000 0 200 1 00 1500 80000 0 100 0 50 Expected Mn conc mg kg Sample amount g Analys...

Страница 85: ...analysis volume from table Expected Ni conc mg kg Sample amount g Analysis Volume mL 4 220 0 500 20 0 10 580 0 400 10 0 25 1500 0 300 5 00 200 11000 0 200 1 00 750 45000 0 100 0 50 Expected Nitrogen c...

Страница 86: ...ed PO4 conc mg kg Sample amount g Analysis Volume mL 10 450 0 500 20 0 25 1100 0 400 10 0 67 3100 0 300 5 00 500 23000 0 200 1 00 2000 93000 0 100 0 50 Expected K conc mg kg Sample amount g Analysis V...

Страница 87: ...onc mg kg Sample amount g Analysis Volume mL 6 300 0 500 20 0 15 750 0 400 10 0 40 2000 0 300 5 0 300 15000 0 200 1 00 1200 60000 0 100 0 50 Expected Zn conc mg kg Sample amount g Analysis Volume mL 1...

Страница 88: ...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 th...

Страница 89: ...80 400 688 9809 www mamots com 0431 85178766...

Страница 90: ...3125 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 fe...

Страница 91: ...82 400 688 9809 www mamots com 0431 85178766...

Страница 92: ...mpany customer service is an important part of every product we make With that in mind we have compiled the following information for your convenience GENERAL INFORMATION 400 688 9809 www mamots com 0...

Страница 93: ...84 400 688 9809 www mamots com 0431 85178766...

Страница 94: ...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...

Страница 95: ...kg 14738 00 pH paper pH 1 11 5 roll pkg 391 33 Pipet Pasteur disposable 229 mm 200 pkg 21234 01 sension 1 Basic Portable pH Meter with electrode each 51700 10 Spatula stainless 10 cm each 561 64 Spoon...

Страница 96: ...87 HOW TO ORDER 400 688 9809 www mamots com 0431 85178766...

Страница 97: ...88 REPAIR SERVICE 400 688 9809 www mamots com 0431 85178766...

Страница 98: ...89 WARRANTY 400 688 9809 www mamots com 0431 85178766...

Страница 99: ...400 688 9809 www mamots com 0431 85178766...

Страница 100: ...400 688 9809 www mamots com 0431 85178766...

Страница 101: ...400 688 9809 www mamots com 0431 85178766...

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