Hach DR2010 User manual

49300-22
DR/2010
SPECTROPHOTOMETER
PROCEDURES MANUAL
© Hach Company, 1996–2000. All rights reserved. Printed in the U.S.A. ap/dk 12/99 7ed
jnb/dk 10/00 rev2
2
TABLE OF CONTENTS
Sample Procedure Explained .................................................................................................. 13
SECTION I CHEMICAL ANALYSIS INFORMATION......................................... 17
Abbreviations .......................................................................................................................... 17
Converting Chemical Species ................................................................................................. 18
Hardness Conversion ........................................................................................................... 19
Dissolved Oxygen................................................................................................................ 20
Sample Collection, Preservation and Storage ...................................................................... 22
Collecting Water Samples ................................................................................................ 25
Acid Washing Bottles....................................................................................................... 25
Correcting for Volume Additions ........................................................................................ 26
Boiling Aids ......................................................................................................................... 26
Sample Filtration.................................................................................................................. 27
Temperature Considerations ................................................................................................ 29
Sample Dilution Techniques................................................................................................ 29
Sample Dilution and Interfering Substances .................................................................... 30
Using Pipets and Graduated Cylinders ................................................................................ 31
Using the TenSette Pipet...................................................................................................... 32
Operating the TenSette Pipet............................................................................................ 32
Mixing Water Samples ........................................................................................................ 33
Using Sample Cells.............................................................................................................. 35
Orientation of Sample Cells.............................................................................................. 35
Care of Hach 1-inch Sample Cells.................................................................................... 35
Cleaning Sample Cells...................................................................................................... 35
Sample Cell Matching ...................................................................................................... 36
Volume Measurement Accuracy ...................................................................................... 37
Using AccuVac Ampuls ...................................................................................................... 37
Using Reagent Powder Pillows............................................................................................ 38
Using PermaChem Pillows .................................................................................................. 39
Using the Pour-Thru Cell..................................................................................................... 39
Reagent and Standard Stability............................................................................................ 40
Interferences............................................................................................................................ 41
pH Interference .................................................................................................................... 41
Accuracy and Precision........................................................................................................... 42
Standard Additions............................................................................................................... 43
3
TABLE OF CONTENTS, continued
Method Performance............................................................................................................... 50
Estimated Detection Limit................................................................................................... 50
Precision .............................................................................................................................. 53
Estimating Precision......................................................................................................... 53
Selecting the Best Wavelength ............................................................................................... 54
Adapting HACH Procedures to Other Spectrophotometers................................................... 57
Preparing a Calibration Curve............................................................................................. 57
%T Versus Concentration Calibration ............................................................................. 57
Absorbance Versus Concentration Calibration ................................................................ 59
USEPA Approved and Accepted Definitions ......................................................................... 60
SECTION II SAMPLE PRETREATMENT ............................................................... 61
Digestion................................................................................................................................. 61
EPA Mild Digestion with Hot Plate for Metals Analysis Only........................................... 61
EPA Vigorous Digestion with Hot Plate for Metals Analysis Only ................................... 62
General Digesdahl Digestion (Not USEPA accepted) ........................................................ 63
Distillation .............................................................................................................................. 63
SECTION III WASTE MANAGEMENT AND SAFETY........................................ 65
Waste Management................................................................................................................. 65
Waste Minimization ............................................................................................................ 65
Regulatory Overview........................................................................................................... 65
Hazardous Waste Definition................................................................................................ 66
Characteristic Hazardous Waste Codes ............................................................................... 67
How to Determine if Waste is Hazardous ........................................................................... 67
Examples of Hazardous Waste............................................................................................ 68
Hazardous Waste Disposal.................................................................................................. 68
Management of Specific Wastes ......................................................................................... 69
Special Considerations for Cyanide Containing Materials .............................................. 69
Resources............................................................................................................................. 70
Material Safety Data Sheets.................................................................................................... 71
How to Obtain an MSDS..................................................................................................... 71
Sections of an MSDS........................................................................................................... 72
4
TABLE OF CONTENTS, continued
Safety....................................................................................................................................... 74
Material Safety Data Sheet .................................................................................................. 74
Reading Labels Carefully .................................................................................................... 74
Protective Equipment........................................................................................................... 75
First Aid Equipment and Supplies ....................................................................................... 75
General Safety Rules............................................................................................................ 75
OSHA Chemical Hygiene Plan............................................................................................ 76
SECTION IV PROCEDURES ........................................................................................ 77
ALUMINUM, Aluminon Method........................................................................................... 79
ALUMINUM, Eriochrome Cyanine R Method...................................................................... 87
ARSENIC, Silver Diethyldithiocarbamate Method ................................................................ 95
BARIUM, Turbidimetric Method ......................................................................................... 103
BENZOTRIAZOLE, UV Photolysis Method ....................................................................... 111
BORON, Carmine Method.................................................................................................... 117
BORON, Low Range, Azomethine-H Method .................................................................... 121
BROMINE, DPD Method..................................................................................................... 129
CADMIUM, Dithizone Method............................................................................................ 137
CHLORIDE, Mercuric Thiocyanate Method........................................................................ 145
CHLORINE, FREE, DPD Method ....................................................................................... 149
CHLORINE, FREE, DPD Rapid Liquid Method ................................................................ 157
CHLORINE, FREE, HIGH RANGE, DPD Method............................................................. 163
CHLORINE, FREE, DPD Test ‘N Tube™ Method ............................................................. 169
CHLORINE, TOTAL, Ultra Low Range, DPD Method ...................................................... 175
CHLORINE, TOTAL, Ultra Low Range, DPD Method ..................................................... 183
CHLORINE, TOTAL, DPD Method .................................................................................... 191
CHLORINE, TOTAL, DPD Rapid Liquid Method ............................................................. 199
CHLORINE, TOTAL, HIGH RANGE, DPD Method ........................................................ 205
CHLORINE, TOTAL, DPD Test ‘N Tube™ Method.......................................................... 211
CHLORINE DIOXIDE, LR, Chlorophenol Red Method..................................................... 217
CHLORINE DIOXIDE, HR, Direct Reading Method.......................................................... 221
CHLORINE DIOXIDE, DPD Method.................................................................................. 223
5
TABLE OF CONTENTS, continued
CHROMIUM, HEXAVALENT, 1,5-Diphenylcarbohydrazide Method.............................. 233
CHROMIUM, TOTAL, Alkaline Hypobromite Oxidation Method ................................... 239
COBALT, 1-(2-Pyridylazo)-2-Naphthol (PAN) Method ..................................................... 245
COLOR, NCASI 253, Platinum-Cobalt Method.................................................................. 249
COLOR, TRUE AND APPARENT, APHA Platinum-Cobalt Standard Method ............... 253
COPPER, Bicinchoninate Method........................................................................................ 257
COPPER, Porphyrin Method................................................................................................ 265
COPPER, AUTOCATALYTIC, Colorimetric Method........................................................ 271
CYANIDE, Pyridine-Pyrazalone Method ............................................................................ 277
CYANURIC ACID, Turbidimetric Method......................................................................... 287
FLUORIDE, SPADNS Method............................................................................................ 291
FORMALDEHYDE, MBTH Method .................................................................................. 299
HARDNESS, Calcium and Magnesium; Calmagite Colorimetric Method.......................... 303
HARDNESS, TOTAL, Ultra Low Range, Calcium and Magnesium Chlorophosphonazo
Colorimetric Method ......................................................................................................... 309
HARDNESS, TOTAL, Ultra Low Range, Calcium and Magnesium; Chlorophosphonazo
Rapid Liquid Method ........................................................................................................ 313
HYDRAZINE, p-Dimethylaminobenzaldehyde Method ..................................................... 319
IODINE, DPD Method ......................................................................................................... 325
IRON, FerroZine Method ..................................................................................................... 333
IRON, FerroZine Rapid Liquid Method............................................................................... 339
IRON, FERROUS, 1,10 Phenanthroline Method................................................................. 345
IRON, TOTAL, FerroMo™ Method.................................................................................... 349
IRON, TOTAL, FerroVer Method ....................................................................................... 353
IRON, TOTAL, TPTZ Method............................................................................................. 361
LEAD, Dithizone Method..................................................................................................... 369
LEAD, LeadTrak™ Fast Column Extraction Method.......................................................... 377
MANGANESE, HR, Periodate Oxidation Method .............................................................. 387
MANGANESE, LR, PAN Method....................................................................................... 391
MERCURY, Cold Vapor Mercury Concentration Method.................................................. 397
MOLYBDENUM, MOLYBDATE, HR, Mercaptoacetic Acid Method.............................. 413
MOLYBDENUM, MOLYBDATE, LR, Ternary Complex Method ................................... 421
6
TABLE OF CONTENTS, continued
NICKEL, 1-(2 Pyridylazo)-2-Naphthol (PAN) Method ....................................................... 427
NICKEL, Heptoxime Method............................................................................................... 433
NICKEL, AUTOCATALYTIC, Photometric Method ......................................................... 439
NITRATE, LR, Cadmium Reduction Method...................................................................... 443
NITRATE, MR, Cadmium Reduction Method..................................................................... 449
NITRATE, HR, Cadmium Reduction Method...................................................................... 457
NITRATE, HR, Chromotropic Acid Method, Test ‘N Tube™ ............................................ 465
NITRITE, LR, Diazotization Method ................................................................................... 471
NITRITE, LR, Diazotization, NED Rapid Liquid Method................................................... 477
NITRITE, LR, Test ‘N Tube, Diazotization (Chromotropic Acid) Method......................... 483
NITRITE, HR, Ferrous Sulfate Method................................................................................ 487
NITROGEN, TOTAL, HR, Test ’N Tube™, TNT Persulfate Digestion Method................ 491
NITROGEN, AMMONIA, Nessler Method......................................................................... 499
NITROGEN, AMMONIA, Salicylate Method ..................................................................... 505
NITROGEN, AMMONIA, High Range, Test ’N Tube, Salicylate Method......................... 511
NITROGEN, AMMONIA, Low Range Test ‘N Tube, Salicylate Method .......................... 517
NITROGEN, MONOCHLORAMINE and FREE AMMONIA, Salicylate Method............ 523
NITROGEN, TOTAL, Test ’N Tube, TNT Persulfate Digestion Method ........................... 531
NITROGEN, TOTAL KJELDAHL, Nessler Method .......................................................... 539
NITROGEN, TOTAL INORGANIC, Test ‘N Tube, Titanium Trichloride Reduction ....... 549
ORGANIC CARBON, TOTAL, Low Range, Direct Method.............................................. 557
ORGANIC CARBON, TOTAL, High Range, Direct Method ............................................. 565
ORGANIC MATTER, Dichromate Method......................................................................... 573
OXYGEN, DISSOLVED, LR, Indigo Carmine Method...................................................... 579
OXYGEN, DISSOLVED, HR, HRDO Method ................................................................... 583
OXYGEN, DISSOLVED, SHR, Super High Range Method............................................... 587
OXYGEN DEMAND, CHEMICAL, Reactor Digestion Method........................................ 591
Colorimetric Determination, 0 to 150 mg/L COD ............................................................. 593
Colorimetric Determination, 0 to 1,500 and 0 to 15,000 mg/L COD................................ 595
OXYGEN DEMAND, CHEMICAL (COD), Dichromate Reflux Method .......................... 601
Colorimetric Determination............................................................................................... 603
Buret Titration.................................................................................................................... 605
OXYGEN DEMAND, CHEMICAL, Manganese III Digestion Method ............................. 611
7
TABLE OF CONTENTS, continued
OXYGEN DEMAND, CHEMICAL, Manganese III Digestion Method............................. 615
OXYGEN SCAVENGERS, Iron Reduction Method for Oxygen Scavengers .................... 623
OZONE, Indigo Method....................................................................................................... 627
PALLADIUM, N,N'-Dimethyldithiooxamide Method ........................................................ 631
PCB IN SOIL, Immunoassay Method.................................................................................. 635
PHENOLS, 4-Aminoantipyrine Method .............................................................................. 645
PHOSPHONATES, Persulfate UV Oxidation Method........................................................ 651
PHOSPHORUS, REACTIVE, PhosVer 3 Method, Test ’N Tube Procedure ...................... 657
PHOSPHORUS, REACTIVE, (Also called Orthophosphate) Amino Acid Method ........... 663
PHOSPHORUS, REACTIVE, (Also called Orthophosphate) Molybdovanadate Method.. 669
PHOSPHORUS, REACTIVE, PhosVer 3 (Ascorbic Acid) Method.................................... 677
PHOSPHORUS, REACTIVE, LOW RANGE, Ascorbic Acid Rapid Liquid Method........ 685
PHOSPHORUS, REACTIVE, HIGH RANGE, Molybdovanadate Rapid Liquid Method . 691
PHOSPHORUS, REACTIVE, HR, Molybdovanadate Method, Test ’N Tube™ ............... 697
PHOSPHORUS, TOTAL, Acid Persulfate Digestion Method............................................. 703
PHOSPHORUS, TOTAL, PhosVer 3 with Acid Persulfate Digestion Test ‘N Tube.......... 707
PHOSPHORUS, TOTAL, HR, Molybdovanadate Method with Acid Persulfate Digestion,
Test ’N Tube™.................................................................................................................. 715
PHOSPHORUS, ACID HYDROLYZABLE, PhosVer3 with Acid Hydrolysis,................. 723
Test ’N Tube...................................................................................................................... 723
PHOSPHORUS, ACID HYDROLYZABLE, Hydrolysis to Orthophosphate Method........ 729
POLYACRYLIC ACID, Absorption-Colorimetric Method ................................................ 733
POTASSIUM, Tetraphenylborate Method........................................................................... 741
QUATERNARY AMMONIUM COMPOUNDS, Direct Binary Complex Method ........... 747
SELENIUM, Diaminobenzidine Method ............................................................................. 753
SILICA, HR, Silicomolybdate Method ................................................................................ 761
SILICA, LR, Heteropoly Blue Method ................................................................................ 767
SILICA, ULTRA LOW RANGE, Heteropoly Blue Method ............................................... 773
SILICA, ULR, Heteropoly Blue Rapid Liquid Method ....................................................... 779
SILVER, Colorimetric Method............................................................................................. 785
SODIUM CHROMATE, Direct Colorimetric Method ........................................................ 791
8
TABLE OF CONTENTS, continued
SULFATE, SulfaVer 4 Method ............................................................................................ 795
SULFIDE, Methylene Blue Method* ................................................................................... 803
SURFACTANTS, ANIONIC, Crystal Violet Method.......................................................... 807
SUSPENDED SOLIDS, Photometric Method...................................................................... 811
TANNIN AND LIGNIN, Tyrosine Method ......................................................................... 815
THM Plus™: Trihalomethanes, ........................................................................................... 819
TOXTRAK TOXICITY TEST, Colorimetric Method ......................................................... 829
TPH IN SOIL, Immunoassay Method................................................................................... 835
TPH IN WATER, Immunoassay Method ............................................................................. 845
TURBIDITY, Attenuated Radiation Method (direct reading) .............................................. 853
VOLATILE ACIDS, Esterification Method......................................................................... 857
ZINC, Zincon Method........................................................................................................... 861
SECTION V GENERAL INFORMATION ............................................................... 867
HOW TO ORDER............................................................................................................ 869
REPAIR SERVICE .......................................................................................................... 870
WARRANTY ..................................................................................................................... 871
9
10

INTRODUCTION

This manual is divided into five sections:
Section I Chemical Analysis Information
This section applies to all the procedures. It provides background information and reference/review material for the technician or chemist. Commonly used techniques are explained in detail.
Section II Sample Pretreatment
This section provides a brief overview of sample pretreatment and three digestion procedures. Two are USEPA digestions. The Hach Digesdahl method is also included.
Section III Waste Management and Safety
Section 3 includes information an waste management, regulations, waste disposal and resources on waste management. The Safety portion covers reading an MSDS and general safety guidelines.
Section IV Procedures
Section 4 contains step-by-step illustrated instructions for measuring over 120 parameters. The steps also include helpful notes. Each procedure contains information on sample collection, storage and preservation, accuracy checks, possible interferences, summary of method and a list of the reagents and apparatus necessary to run the test.
Section V Ordering Information
This section provides information needed for ordering, shipping, return of items and Hach trademarks.
Before attempting the analysis procedures the analyst should read the instrument manual to learn about the spectrophotometer’s features and operation.
11
INTRODUCTION, continued
Hach Company Trademarks
AccuGrow
AccuVac
AccuVer
AccuVial
Add-A-Test
AgriTrak
AluVer
AmVer
APA 6000
AquaChek
AquaTrend
BariVer
BODTrak
BoroTrace
BoroVer
C. Moore Green
CA 610
CalVer
ChromaVer
ColorQuik
CoolTrak
CuVer
CyaniVer
Digesdahl
DithiVer
Dr. F. Fluent
Dr. H. Tueau
DR/Check
EC 310
FerroMo
FerroVer
FerroZine
FilterTrak 660
Formula 2533
Formula 2589
Gelex
®
®
®
®
®
®
®
®
®
®
®
®
®
®
®
®
®
®
H2O University
H2OU
Hach Logo
Hach One
Hach Oval
Hach.com
HachLink
Hawkeye The Hach Guy
HexaVer
HgEx
HydraVer
ICE-PIC
IncuTrol
Just Add Water
LeadTrak
M-ColiBlue24
ManVer
MolyVer
Mug-O-Meter
NetSketcher
NitraVer
NitriVer
NTrak
OASIS
On Site Analysis. Results You Can Trust
OptiQuant
OriFlow
OxyVer
PathoScreen
PbEx
PermaChem
PhosVer
Pocket Colorimeter
Pocket Pal
Pocket Turbidimeter
®
®
®
®
®
®
®
®
®
®
®
®
®
®
SM
®
®
®
Pond In Pillow
®
ion
®
®
®
®
SM
®
®
®
®
®
®
SM
®
®
®
®
PourRite
PrepTab
ProNetic
Pump Colorimeter
QuanTab
Rapid Liquid
RapidSilver
Ratio
RoVer
sens
Simply Accurate
SINGLET
SofChek
SoilSYS
SP 510
Spec
StablCal
StannaVer
SteriChek
StillVer
SulfaVer
Surface Scatter
TanniVer
TenSette
Test N Tube
TestYES!
TitraStir
TitraVer
ToxTrak
UniVer
VIScreen
Voluette
WasteAway
ZincoVer
12
Sample Procedure Explained
13
Sample Procedure Explained, continued
14
Sample Procedure Explained, continued
15
16

SECTION I CHEMICAL ANALYSIS INFORMATION

Abbreviations
The following abbreviations are used throughout the text of the procedure section:
Abbrev-
iation
°C degree(s) Celsius (Centigrade) HR high range
°F degree(s) Fahrenheit kg/ha kilograms per hectare
ACS
APHA Standard Methods
AV AccuVac MR medium range
Bicn bicinchoninate NIPDWR
CFR Code of Federal Regulations NPDES
conc concentrated P phosphorus
DB dropping bottle PCB Poly chlorinated biphenyl
EDL Estimated detection limit PV PhosVer
F&T free and total RL Rapid Liquid
FAU
FM FerroMo
FV FerroVer
FZ FerroZine
gr/gal grains per gallon (1 gr/gal = 17.12 mg/L) USEPA
American Chemical Society reagent grade purity
Standard Methods for the Examination of Water and Wastewater, published jointly by
the American Public Health Association (APHA), the American Water Works Association (AWWA), and the Water Environment Federation (WEF). Order from Hach requesting Cat. No. 22708-00 or from the Publication Office of the American Public Health Association. This book is the standard reference work for water analysis. Many procedures contained in this manual are based on Standard Methods.
Formazin Attenuation Units. Turbidity unit of measure based on a Formazin stock suspension.
g grams ULR Ultra low range
Definition
®
®
®
Abbrev-
iation
l or L
lbs/Ac pounds per acre
LR low range
MDL Method detection limit
MDB marked dropping bottle
mg/L milligrams per liter (ppm)
µg/L micrograms per liter (ppb)
ml or mL
SCDB self-contained dropping bottle
TNT Te s t N Tube
TPH Total petroleum hydrocarbons
TPTZ (2,4,6-Tri-(2-Pyridyl)-1,3,5-Triazine)
Liter. Volume equal to one cubic decimeter (dm
(milliliter)-approximately the same as a cubic centimeter (cc) or 1/1000 of a liter. Also known as a “cc”.
National Interim Primary Drinking Water Regulations
National Pollutant Discharge Elimination System
United States Environmental Protection Agency
®
Definition
3
)
17
SECTION I, continued
Converting Chemical Species
Species conversion factors for many commonly used substances are preprogrammed into the DR/2010 (see Table 1). Conversions are method specific and are viewable after taking the reading by pressing
Table 1 Conversion Factors
To Convert From... To... Multiply By... Conversion used in program #
mg/L Al mg/L Al2O
mg/L B mg/L H
mg/L Ca-CaCO
mg/L CaCO
mg/L CaCO
3
3
3
3BO3
mg/L Ca 0.4004 220
mg/L Ca 0.4004 227
mg/L Mg 0.2428 227
3
1.8895 9, 10
5.7 45
µg/L Carbo. µg/L Hydro. 1.92 182
µg/L Carbo. µg/L ISA 2.69 182
µg/L Carbo. µg/L MEKO 3.15 182
mg/L Cr
mg/L Cr
mg/L Mg-CaCO
6+
6+
3
mg/L CrO
mg/L Na2CrO
mg/L Mg 0.2428 225
mg/L Mn mg/L KMnO
mg/L Mn mg/L MnO
mg/L Mo
mg/L Mo
6+
6+
mg/L MoO
mg/L Na2MoO
mg/L N mg/L NH
mg/L N mg/L NO
mg/L Na
mg/L Na
mg/L NH
mg/L NH
mg/L NH
mg/L NH
mg/L NO
mg/L NO
mg/L NO
µg/L NO
mg/L NO
µg/L NO
mg/L NO
mg/L PO
µg/L PO
mg/L PO
µg/L PO
mg/L SiO
µg/L SiO
CrO
2
4
CrO
2
4
Cl-N mg/L Cl
2
Cl-N mg/L NH2Cl 3.6750 386
2
-N mg/L NH
3
-N mg/L NH
3
-
2
-
2
-
-N mg/L NaNO
2
-
-N µg/L NaNO
2
-
-N mg/L NO
2
-
-N µg/L NO
2
-
-N mg/L NO
3
3-
4
3-
4
3-
4
3-
4
2
2
mg/L Cr
mg/L CrO
mg/L NaNO
mg/L NO
mg/L P 0.3261 480, 482, 485, 490, 492, 535
µg/L P 0.3261 488
mg/L P2O
µg/L P2O
mg/L Si 0.4674 651, 656
µg/L Si 0.4674 645
2-
4
4
4
-
4
2-
4
4
3
-
3
6+
2-
4
2
3
+
4
2
-
-N 0.3045 373
2
2
2
-
2
-
2
-
3
5
5
2.231 90, 95
3.115 90, 95
2.876 290, 295
2.165 290, 295
1.667 315, 320, 322
2.146 315, 320, 322
1.216 342, 343, 346, 347, 348
4.427 346, 347, 348
0.321 670
0.72 670
5.0623 386
1.216 380, 385, 387
1.288 380, 385, 387
1.5 373
4.926 345, 371, 375
4.926 376
3.284 345, 371, 375
3.284 376
4.427 344, 351, 353, 355, 359, 361
0.7473 480, 482, 485, 490, 492, 535
0.7473 488
18
CONC.
SECTION I, continued
Hardness Conversion
Table 2 lists the factors for converting one unit of measure for hardness to another unit of measure. For example, to convert mg/L CaCO parts/100,000 CaO, multiply the value in mg/L x 0.056.
Table 2 Hardness Conversion Factors
Units of
Measure
mg/L
CaCO
English
British
3
gr/gal
(Imperial)
mg/L
CaCO
CaCO
1.0 0.07 0.058 0.1 0.056 0.02 5.6x10
3
14.3 1.0 0.83 1.43 0.83 0.286 8.0x10
3
American
gr/gal (US)
CaCO
gr/gal
CaCO
3
US gr/gal
CaCO
Fr. p/
17.1 1.2 1.0 1.72 0.96 0.343 9.66x10
3
10.0 0.7 0.58 1.0 0.56 0.2 5.6x10
100,000
CaCO
3
Ger. p/
17.9 1.25 1.04 1.79 1.0 0.358 1x10
100,000
CaO
meq/L 50.0 3.5 2.9 5.0 2.8 1.0 2.8x10
g/L CaO 1790.0 125.0 104.2 179.0 100.0 35.8 1.0 0.112
lbs./cu ft
CaCO
16,100.0 1,123.0 935.0 1,610.0 900.0 321.0 9.0 1.0
3
1 epm/L, or mval/L
Note: 1 meq/L = 1N/1000
French
parts/
100,000
3
CaCO
3
German
Parts/
100,000
CaO
meq/L
1
g/L CaO
to German
3
lbs./cu ft
-4
6.23x10
-3
-3
1.07x10
-3
6.23x10
-2
1.12x10
-2
3.11x10
CaCO
8.9x10
3
-5
-4
-3
-4
-3
-2
19
SECTION I, continued
Dissolved Oxygen
Table 3 lists the mg/L dissolved oxygen in water at saturation for various temperatures and atmospheric pressures. The table was formulated in a laboratory using pure water. The values given are only approximations for estimating the oxygen content of a particular body of surface water.
Table 3 Dissolved Oxygen Saturation in Water
Pressure in Millimeters and Inches Hg
mm
775 760 750 725 700 675 650 625
Temp inches
°F °C 30.51 29.92 29.53 28.45 27.56 26.57 25.59 24.61
32.0 0 14.9 14.6 14.4 13.9 13.5 12.9 12.5 12.0
33.8 1 14.5 14.2 14.1 13.6 13.1 12.6 12.2 11.7
35.6 2 14.1 13.9 13.7 13.2 12.9 12.3 11.8 11.4
37.4 3 13.8 13.5 13.3 12.9 12.4 12.0 11.5 11.1
39.2 4 13.4 13.2 13.0 12.5 12.1 11.7 11.2 10.8
41.0 5 13.1 12.8 12.6 12.2 11.8 11.4 10.9 10.5
42.8 6 12.7 12.5 12.3 11.9 11.5 11.1 10.7 10.3
44.6 7 12.4 12.2 12.0 11.6 11.2 10.8 10.4 10.0
46.4 8 12.1 11.9 11.7 11.3 10.9 10.5 10.1 9.8
48.2 9 11.8 11.6 11.5 11.1 10.7 10.3 9.9 9.5
50.0 10 11.6 11.3 11.2 10.8 10.4 10.1 9.7 9.3
51.8 11 11.3 11.1 10.9 10.6 10.2 9.8 9.5 9.1
53.6 12 11.1 10.8 10.7 10.3 10.0 9.6 9.2 8.9
55.4 13 10.8 10.6 10.5 10.1 9.8 9.4 9.1 8.7
57.2 14 10.6 10.4 10.2 9.9 9.5 9.2 8.9 8.5
59.0 15 10.4 10.2 10.0 9.7 9.3 9.0 8.7 8.3
60.8 16 10.1 9.9 9.8 9.5 9.1 8.8 8.5 8.1
62.6 17 9.9 9.7 9.6 9.3 9.0 8.6 8.3 8.0
64.4 18 9.7 9.5 9.4 9.1 8.8 8.4 8.1 7.8
66.2 19 9.5 9.3 9.2 8.9 8.6 8.3 8.0 7.6
68.0 20 9.3 9.2 9.1 8.7 8.4 8.1 7.8 7.5
69.8 21 9.2 9.0 8.9 8.6 8.3 8.0 7.7 7.4
71.6 22 9.0 8.8 8.7 8.4 8.1 7.8 7.5 7.2
73.4 23 8.8 8.7 8.5 8.2 8.0 7.7 7.4 7.1
75.2 24 8.7 8.5 8.4 8.1 7.8 7.5 7.2 7.0
77.0 25 8.5 8.4 8.3 8.0 7.7 7.4 7.1 6.8
78.8 26 8.4 8.2 8.1 7.8 7.6 7.3 7.0 6.7
80.6 27 8.2 8.1 8.0 7.7 7.4 7.1 6.9 6.6
20
SECTION I, continued
Table 3 Dissolved Oxygen Saturation in Water (continued)
Pressure in Millimeters and Inches Hg
mm
775 760 750 725 700 675 650 625
Temp inches
°F °C 30.51 29.92 29.53 28.45 27.56 26.57 25.59 24.61
82.4 28 8.1 7.9 7.8 7.6 7.3 7.0 6.7 6.5
84.2 29 7.9 7.8 7.7 7.4 7.2 6.9 6.6 6.4
86.0 30 7.8 7.7 7.6 7.3 7.0 6.8 6.5 6.2
87.8 31 7.7 7.5 7.4 7.2 6.9 6.7 6.4 6.1
89.6 32 7.6 7.4 7.3 7.0 6.8 6.6 6.3 6.0
91.4 33 7.4 7.3 7.2 6.9 6.7 6.4 6.2 5.9
93.2 34 7.3 7.2 7.1 6.8 6.6 6.3 6.1 5.8
95.0 35 7.2 7.1 7.0 6.7 6.5 6.2 6.0 5.7
96.8 36 7.1 7.0 6.9 6.6 6.4 6.1 5.9 5.6
98.6 37 7.0 6.8 6.7 6.5 6.3 6.0 5.8 5.6
100.4 38 6.9 6.7 6.6 6.4 6.2 5.9 5.7 5.5
102.2 39 6.8 6.6 6.5 6.3 6.1 5.8 5.6 5.4
104.0 40 6.7 6.5 6.4 6.2 6.0 5.7 5.5 5.3
105.8 41 6.6 6.4 6.3 6.1 5.9 5.6 5.4 5.2
107.6 42 6.5 6.3 6.2 6.0 5.8 5.6 5.3 5.1
109.4 43 6.4 6.2 6.1 5.9 5.7 5.5 5.2 5.0
111.2 44 6.3 6.1 6.0 5.8 5.6 5.4 5.2 4.9
113.0 45 6.2 6.0 5.9 5.7 5.5 5.3 5.1 4.8
114.8 46 6.1 5.9 5.9 5.6 5.4 5.2 5.4 4.8
116.6 47 6.0 5.9 5.8 5.6 5.3 5.1 4.8 4.7
118.4 48 5.9 5.8 5.7 5.5 5.3 5.0 4.8 4.6
120.2 49 5.8 5.7 5.6 5.4 5.2 5.0 4.7 4.5
122.0 50 5.7 5.6 5.5 5.3 5.1 4.9 4.7 4.4
21
SECTION I, continued
Sample Collection, Preservation and Storage
Correct sampling and storage are critical for accurate testing. For greatest accuracy, thoroughly clean sampling devices and containers to prevent carryover from previous samples. Preserve the sample properly; each procedure has information about sample preservation.
The least expensive containers are polypropylene or polyethylene.
The best and most expensive containers are quartz or PTFE
(polytetrafluoroethylene, Teflon).
Avoid soft glass containers for metals in the
microgram-per-liter range.
Store samples for silver determination in light absorbing containers,
such as amber bottles.
Avoid contaminating the sample with metals from containers, distilled water or membrane filters. Thoroughly clean sample containers as described under Acid Washing Bottles.
Preservation slows the chemical and biological changes that continue after collection. These changes may change the amount of a chemical species available for analysis. Normally, analyze the samples as soon as possible after collection, especially when the analyte concentration is expected to be low. This also reduces the chance for error and minimizes labor.
Preservation methods include pH control, chemical addition, refrigeration and freezing. Table 4 gives the recommended preservation for various substances. It also includes suggested types of containers and the maximum recommended holding times for properly preserved samples.
Preserve aluminum, cadmium, chromium, cobalt, copper, iron, lead, nickel, potassium, silver and zinc samples for at least 24 hours by adding one Nitric Acid Solution Pillow 1:1 (Cat. No. 2540-98) per liter of sample. Check the pH with pH indicator paper or a pH meter to assure the pH is 2 or less. Add additional pillows if necessary. Adjust the sample pH prior to analysis by adding an equal number of Sodium Carbonate Anhydrous Powder Pillows (Cat. No. 179-98). Or raise the pH to 4.5 with Sodium Hydroxide Standard Solution, 1 N or 5 N.
22
SECTION I, continued
Table 4 Required Containers, Preservation Techniques and Holding Times
Parameter No./Name Container
2
Preservation
3,4
1
Maximum
Holding Time
5
Table 1A - Bacterial Tests
1-4. Coliform, fecal and total P,G Cool, 4°C, 0.008%, Na
5. Fecal streptococci P,G Cool, 4°C, 0.008%, Na
2S2O3
2S2O3
6
6
6 hours
6 hours
Table 1B - Inorganic Tests
1. Acidity P, G Cool, 4°C 14 days
2. Alkalinity P, G Cool, 4°C 14 days
4. Ammonia P, G Cool, 4°C, H
9. Biochemical oxygen demand
P, G Cool, 4°C 48 hours
to pH<2 28 days
2SO4
(BOD)
10. Boron P, PFTE or quartz HNO
to pH<2 6 months
3
11. Bromide P, G None required 28 days
14. Biochemical oxygen demand,
P, G Cool, 4°C 48 hours
carbonaceous
15. Chemical oxygen demand P, G Cool, 4°C, H
to pH<2 28 days
2SO4
16. Chloride P, G None required 28 days
17. Chlorine, total residual P, G None required Analyze immediately
21. Color P, G Cool, 4°C 48 hours
23-24. Cyanide, total and amenable to chlorination
P, G Cool, 4°C, NaOH to pH>12, 0.6 g
ascorbic acid
6
14 days
7
25. Fluoride P None required 28 days
27. Hardness P, G HNO
to pH<2, H2SO4 to pH<2 6 months
3
28. Hydrogen ion (pH) P, G None required Analyze immediately
31, 43. Kjeldahl and organic
P, G Cool 4°C, H
to pH<2 28 days
2SO4
nitrogen
8
Metals
18. Chromium VI P, G Cool, 4°C 24 hours
35. Mercury P, G HNO
to pH<2 28 days
3
Metals, except boron, chromium VI and mercury: 3, 5-8, 12, 13, 19, 20, 22, 26, 29, 30, 32-34, 36, 37, 45, 47, 51, 52, 58-60, 62, 63, 70-72, 74,
9
.
75
P, G HNO
to pH<2 6 months
3
38. Nitrate P, G Cool, 4°C 48 hours
39. Nitrate-nitrite P, G Cool 4°C, H
to pH<2 28 days
2SO4
40. Nitrite P, G Cool, 4°C 48 hours
41. Oil and grease G Cool, 4°C, HCl or H
42. Organic Carbon
P, G Cool, 4°C, HCl or H
to pH<2
H
3PO4
to pH<2 28 days
2SO4
SO4 or
2
28 days
44. Orthophosphate P, G Filter immediately; Cool, 4°C 48 hours
46a. Oxygen, dissolved probe G Bottle and top None required Analyze immediately
46b. Oxygen, dissolved, Winkler Do Fix on site and store in dark 8 hours
48. Phenols G only Cool 4°C, H
to pH<2 28 days
2SO4
23
SECTION I, continued
Table 4 Required Containers, Preservation Techniques and Holding Times1 (continued)
Parameter No./Name Container
49. Phosphorus, elemental G Cool, 4°C 48 hours
50. Phosphorus, total P, G Cool, 4°C, H
53. Residue, total P, G Cool, 4°C7 days
54. Residue, filterable P, G Cool, 4°C7 days
55. Residue, Nonfilterable (TSS) P, G Cool, 4°C7 days
56. Residue, Settleable P, G Cool, 4°C 48 hours
57. Residue, volatile P, G Cool, 4°C7 days
61. Silica P, PFTE or quartz Cool, 4°C 28 days
64. Specific conductance P, G Cool, 4°C 28 days
65. Sulfate P, G Cool, 4°C 28 days
66. Sulfide
67. Sulfite P, G none required Analyze immediately
68. Surfactants P, G Cool, 4°C 48 hours
69. Temperature P, G None required Analyze immediately
73. Turbidity P, G Cool, 4°C 48 hours
1 This table was adapted from Table II published in the Federal Register, July 1, 1997, 40 CFR, Part 136.3,
pages 26-27. Organic tests are not included. 2 Polyethylene (P) or glass (G). 3 Sample preservation should be performed immediately upon sample collection. For composite chemical samples
each aliquot should be preserved at the time of collection. When use of an automated sampler makes it impossible
to preserve each aliquot, then chemical samples may be preserved by maintaining at 4°C until compositing and
sample splitting is completed. 4 When any sample is to be shipped by common carrier or sent through United States Mails, it must comply with the
Department of Transportation Hazardous Material Regulations (49 CFR Part 172). The person offering such
material for transportation is responsible for ensuring such compliance. For the preservation requirements of Table
II, the Office of Hazardous Materials, Materials Transportation Bureau, Department of Transportation has
determined that the Hazardous Materials Regulations do not apply to the following materials: Hydrochloric acid
(HCl) in water solutions at concentrations of 0.04% by weight or less (pH about 1.96 or greater); Nitric acid (HNO
in water solutions at concentrations of 0.15% by weight or less (pH about 1.62 or greater); Sulfuric acid (H
water solutions at concentrations of 0.35% by weight or less (pH about 1.15 or greater); and Sodium hydroxide
(NaOH) in water solutions at concentrations of 0.080% by weight or less (pH about 12.30 or less). 5 Samples should be analyzed as soon as possible after collection. The times listed are the maximum times that
samples may be held before analysis and still be considered valid. Samples may be held for longer periods only if
the permitee, or monitoring laboratory, has data on file to show that the specific types of samples under study are
stable for the longer time, and has received a variance from the Regional Administer under §136.3(e). Some
samples may not be stable for the maximum time period given in the table. A permitee, or monitoring laboratory, is
obligated to hold the sample for a shorter time if knowledge exists to show that this is necessary to maintain sample
stability. See §136.3(e) for details. The term analyze immediately usually means within 15 minutes or less after
sample collection. 6 Should only be used in the presence of residual chlorine. 7 Maximum holding time is 24 hours when sulfide is present. Optionally all samples may be tested with lead acetate
paper before pH adjustments in order to determine if sulfide is present. If sulfide is present, it can be removed by the
addition of cadmium nitrate powder until a negative spot test is obtained. The sample is filtered and then NaOH is
added to pH 12. 8 Samples should be filtered immediately on-site before adding preservative for dissolved metals. 9 Numbers refer to parameter number in 40 CFR, Part 136.3, Table 1B.
2
P, G Cool 4°C, add zinc acetate plus
Preservation
sodium hydroxide to pH>9
3,4
to pH<2 28 days
2SO4
Maximum
Holding Time
7 days
2SO4
5
) in
)
3
24
SECTION I, continued
Collecting Water Samples
Obtain the best sample by careful collection. In general, collect samples near the center of the vessel or duct and below the surface. Use only clean containers (bottles, beakers). Rinse the container several times first with the water to be sampled.
Take samples as close as possible to the source of the supply. This lessens the influence the distribution system has on the sample. Let the water run long enough to flush the system. Fill sample containers slowly with a gentle stream to avoid turbulence and air bubbles. Collect water samples from wells after the pump has run long enough to deliver water representative of the ground water feeding the well.
It is hard to obtain a truly representative sample when collecting surface water samples. Obtain best results by testing several samples. Use samples taken at different times from several locations and depths. The results can be used to establish patterns for that particular body of water.
Generally, as little time as possible should elapse between collecting the sample and analyzing it.
Depending on the test, special precautions in handling the sample may be necessary. This prevents natural interferences such as organic growth or loss or gain of dissolved gases. Each procedure describes sample preservatives and storage techniques for samples that are held for testing.
Acid Washing Bottles
If a procedure suggests acid-washing, use the following procedure:
Use chromic acid or chromium-free substitutes to remove organic deposits from glass containers. Rinse containers thoroughly with water to remove traces of chromium.
a) Clean the glassware or plasticware with laboratory detergent
(phosphate-free detergent is recommended).
b) Rinse well with tap water.
c) Rinse with a 1:1 Hydrochloric Acid Solution or 1:1 Nitric Acid
Solution. The nitric acid rinse is important for testing for lead.
d) Rinse well with deionized water. Up to 12-15 rinses may be
necessary if chromium is being determined.
e) Air dry.
25
SECTION I, continued
Wash glassware for phosphate determinations with phosphate-free detergents and acid-wash with 1:1 HCl. Thoroughly rinse the glassware with deionized water. For ammonia and Kjeldahl nitrogen, rinse with ammonia-free water.
Correcting for Volume Additions
If you use a large volume of preservative, correct for the volume of preservative added. This accounts for dilution due to the acid added to preserve the sample and the base used to adjust the pH to the range of the procedure. This correction is made as follows:
1. Determine the volume of initial sample, the volume of acid and base
added, and the total final volume of the sample.
2. Divide the total volume by the initial volume.
3. Multiply the test result by this factor.
Example:
A one-liter sample was preserved with 2 mL of nitric acid. It was neutralized with 5 mL of 5 N sodium hydroxide. The result of the analysis procedure was 10.00 mg/L. What is the volume correction factor and correct result?
Boiling Aids
Total Volume 1000 mL 2 mL 5 mL++ 1007 mL==
1.
1007
------------- 1.007 volume correction factor==
2.
1000
10.0 mg/L 1.007× 10.07 mg/L correct result==
3.
Hach 1:1 Nitric Acid Pillows contain 2.5 mL of acid: correct for this volume. The addition of a Sodium Carbonate Power Pillow neutralizes the 1:1 Nitric Acid Pillow does not need to be corrected for.
Boiling is necessary in some procedures. Using a boiling aid such as boiling chips (Cat. no. 14835-31) reduces bumping. Bumping is caused by the sudden, almost explosive conversion of water to steam as it is heated. Avoid bumping; it may cause sample loss or injury.
Make sure the boiling aids will not contaminate the sample. Do not use boiling aids (except glass beads) more than once. Loosely covering the sample during boiling will prevent splashing, reduce the chances of contamination and minimize sample loss.
26
SECTION I, continued
Sample Filtration
Filtering separates particles from the aqueous sample. Filtration uses a medium, usually filter paper, to retain particles but pass solution. This is especially helpful when sample turbidity interferes with analysis. Two general methods of filtration are gravity and vacuum. Gravity filtration uses gravity to pull the sample though the filter paper. Vacuum filtration uses suction and gravity to move the sample through the filter. An aspirator or vacuum pump creates the suction. Vacuum filtration is faster than gravity filtration. Vacuum filter (see Figure 1) as follows:
1. Using tweezers, place a filter paper into the filter holder.
2. Place the filter holder assembly in the filtering flask. Wet the filter
with deionized water to ensure adhesion to the holder.
3. Position the funnel housing on the filter holder assembly.
4. While applying a vacuum to the filtering flask, transfer the sample to
the filtering apparatus.
5. Slowly release the vacuum from the filtering flask and transfer the
solution from the filter flask to another container.
Figure 1 Vacuum Filtration
REQUIRED APPARATUS FOR VACUUM FILTRATION
Description Unit Cat. No.
Filter Discs, glass 47 mm.................................................................. 100/pkg................2530-00
Filter Holder, membrane ......................................................................... each..............13529-00
Flask, filter, 500 mL ................................................................................ each..................546-49
Pump, vacuum, hand operated ................................................................each..............14283-00
OR
Pump, vacuum, portable, 115 V ..............................................................each..............14697-00
Pump, vacuum, portable, 230 V ..............................................................each..............14697-02
27
SECTION I, continued
Many of the procedures in this manual use gravity filtration. The only labware required is filter paper, a conical funnel and a receiving flask. This labware is included under Optional Equipment and Supplies at the end of a procedure. Gravity filtration is better for retaining fine particles. For faster filtering, add solution until the filter paper cone is three-fourths filled. Never fill the cone completely. Gravity filter (see Figure 2) as follows:
1. Place a filter paper into the funnel.
2. Wet the filter with deionized water to ensure adhesion to the funnel.
3. Place the funnel into an erlenmeyer flask or graduated cylinder.
4. Pour the sample into the funnel.
Figure 2 Gravity Filtration
REQUIRED APPARATUS FOR GRAVITY FILTRATION
Description Unit Cat No.
Cylinder, graduated, 100 mL ...................................................................each ................. 508-42
Funnel, poly, 65 mm ................................................................................each ............... 1083-67
Filter Paper, 12.5 cm ................................................................................each ............... 1894-57
Flask, erlenmeyer, 125 mL ......................................................................each ................. 505-43
Testing for metals requires acid and heat to pretreat the sample. Since these conditions destroy filter paper, vacuum filtration with glass fiber filter discs is recommended. Also, glass filter discs, unlike paper, do not retain colored species.
28
SECTION I, continued
Temperature Considerations
For best results, most tests in this manual should be performed with sample temperatures between 20 °C (68 °F) and 25 °C (77 °F). If a test requires closer temperature control, notes in the procedure will indicate this.
Sample Dilution Techniques
Ten and 25 mL are the volumes used for most colorimetric tests. However, in some tests, the color developed in the sample may be too intense to be measured. Unexpected colors may develop in other tests. In both cases, dilute the sample to determine if interfering substances are present.
To dilute the sample easily, pipet the chosen sample portion into a clean graduated cylinder (or volumetric flask for more accurate work). Fill the cylinder (or flask) to the desired volume with deionized water. Mix well. Use the diluted sample when running the test.
To help with dilutions, Table 5 shows the amount of sample used, the amount of deionized water used to bring the volume up to 25 mL and the multiplication factor.
The concentration of the sample is equal to the diluted sample reading multiplied by the multiplication factor.
More accurate dilutions can be done with a pipet and a 100-mL volumetric flask (see Table 6 for more information). Pipet the sample and dilute to volume with deionized water. Swirl to mix.
Table 5 Sample Dilution Volumes
Sample
Volume (mL)
25.0 0.0 1
12.5 12.5 2
1
10.0
1
5.0
1
2.5
1
1.0
1
0.250
1 For sample sizes of 10 mL or less, use a pipet to measure the sample into the graduated
cylinder or volumetric flask.
mL deionized Water Used
to Bring the Volume to 25 mL
15.0 2.5
20.0 5
22.5 10
24.0 25
24.75 100
Multiplication
Factor
29
SECTION I, continued
Table 6 Multiplication Factors for Diluting to 100 mL
Sample Volume (mL) Multiplication Factor
1 100
250
520
10 10
25 4
50 2
Sample Dilution and Interfering Substances
Sample dilution may influence the level at which a substance may interfere. The effect of the interferences decreases as the dilution increases. In other words, higher levels of an interfering substance can be present in the original sample if it is diluted before analysis.
An Example:
Copper does not interfere at or below 100 mg/L for a 25.00 mL sample in a procedure. If the sample volume is diluted with an equal volume of water, what is the level at which copper will not interfere?
Total volume
------------- ----------------- ----------- Dilution factor= Sample volume
25
----------- 2=
12.5
Interference Level Dilution Factor× Interference level in sample=
100 2× 200=
The level at which copper will not interfere in the undiluted sample is at or below 200 mg/L.
30
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