USGS

METHODS FOR DETERMINATION OF INORGANIC SUBSTANCES IN WATER AND FLUVIAL SEDIMENTS

U.S. Geological Survey, Techniques of Water-Resources Investigations, Book 5, Chapter A1

By Marvin J. Fishman and Linda C. Friedman, Editors


Table of Contents

Preface

Contributors

Abstract

Introduction

Purpose

Scope

Definitions

Significant figures

References

Quality control

Accuracy of analysis

Basic laboratory and field requirements

Chemical ionic balance

Relation of residue on evaporation to calculated dissolved solids

Relation of specific conductance to residue on

evaporation

Precision of analysis

Reference materials

The central laboratories

Use and documentation of standard laboratory procedures

Analytical review procedure

References

Laboratory equipment and techniques

Glassware and other containers

Chemicals and solutions

Purity

Standard solutions

Nonstandard solutions

Accuracy of measurement

References

Analytical techniques

Gravimetry

Principles

Analytical balance

Accuracy

Titrimetry

Principles

Standard solutions

Factor-weight computations

Automatic titrations

Atomic absorption spectrometry

Basic principles

Instrumental principles

Radiant energy source

Sample chamber

Wavelength selector

Detector

Information processing

Analytical procedures

Direct

Chelation-extraction

Standard additions

Interferences

Ionization effects

Chemical effects

Matirx effects

Spectral line effects

Background absorption

Automation techniques

References

Atomic emission spectrometry

Principles

Emission phenomenon

Quantitative analysis by emission

Types of excitation sources

Flames

Direct-current arc

Alternating-current spark

Direct-current argon plasma (plasma jet)

Inductively-coupled argon radio frequency plasma torch

References

Calorimetry

Basic principles

Instrumental principles

Analytical procedures

Interferences

Automated analysis

References

Electrometry

Voltammetry

Ion-selective electrodes

Specific inductor

pH

References

Ion chromatography

Principles

Apparatus

Pumps

Sample injection systems

Separator resins

Suppressor resins

Detectors

Automation

References

Sample preparation and pretreatment

Sample preparation, bottom-material

Subsampling, bottom-material, coring

Subsampling, bottom-material, splitting

Percent moisture, total-in-bottom-material, gravimetric

Extraction procedure, bottom-material

Extraction procedure, water-suspended sediment

Total decomposition, sediment

Analytical methods

Acidity, electrometric titration

Alkalinity, electrometric titration

Alkalinity, electrometric titration, automated

Aluminum, atomic emission spectrometric, d-c plasma

Aluminum, atomic absorption spectrometric chelation-extraction

Aluminum, atomic absorption spectrometric, direct

Aluminum, total-in-sediment. atomic absorption spectrometric, direct

Antimony, atomic absorption spectrometric, hydride

Antimony, total-in-sediment, atomic absorption spectrometric, hydride

Arsenic, atomic absorption spectrometric, hydride

Arsenic, atomic absorption spectrometric, hydride, automated

Arsenic, colorimetric, silver sdiethyldithiocarbanate

Arsenic, total-in-sediment, atomic absorption spectrometric, hydride

Barium, atomic absorption spectrometric, direct

Barium, atomic emission spectrometric, ICP

Beryllium, atomic absorption spectrometric direct

Beryllium, atomic emission spectrometric, ICP

Boron, atomic emission spectrometric, d-c plasma

Boron, calorimetric, asomethine H. automated-segmented flow

Boron, calorimetric, curcumin

Boron, calorimetric, dianthrimide

Bromide, titrimetric. hypochlorite oxidation

Bromide, ion-exchange chromatographic, automated

Bromide, ion-exchange chromatographic-electrochemical, automated

Bromide, calorimetric, fluorescein, automated segmented flow

Cadmium, atomic absorption spectrometric, chelation-extraction

Cadmium. atomic absorption spectrometric, direct

Cadmium, atomic absorption spectrometric, graphite furnace

Cadmium. atomic emission spectrometric, ICP

Cadmium, total-in-sediment, atomic absorption spectrometric, direct

Calcium, atomic absorption spectrometric, direct

Calcium, atomic absorption spectrometric, direct-EPA

Calcium, atomic emission spectrometric, ICP

Calcium, totabin-sediment, atomic absorption spectrometric, direct

Carbon dioxide, calculation

Chloride, calorimetric, ferric thiocyanate

Chloride, calorimetric, ferric thiocyanate, automated-segmented flow

Chloride, calorimetric, ferric thiocyanate, automated-discrete

Chloride, titrimetric, mercurimetric

Chloride, titrimetric, Mohr

Chloride, ion-exchange chromatographic, automated

Chromium, atomic absorption spectrometric, chelation-extraction

Chromium, atomic absorption spectrometric, direct

Chromium, atomic absorption spectrometric, graphite furnace

Chromium, total-in-sediment, atomic absorption spectrometric, direct

Chromium, hexavalent, atomic absorption spectrometric, chelation-extraction

Chromium, hexavalent, calorimetric, diphenylcarboxide

Cobalt, atomic absorption spectrometric, chelation-extraction

Cobalt, atomic absorption spectrometric, direct

Cobalt, atomic absorption spectrometric, graphite furnace

Cobalt, atomic emission spectrometric, ICP

Cobalt, total-in-sediment, atomic absorption spectrometric, direct

Color, electrometric, visual comparison

Copper, atomic absorption spectrometric chelation-extraction

Copper, atomic absorption spectrometric, direct

Copper, atomic absorption spectrometric, graphite furnace

Copper, atomic emission spectrometric, ICP

Copper, total-in-sediment, atomic absorption spectrometric, direct

Cyanide, calorimetric, barbituric acid, automated-segmented flow

Cyanide, calorimetric, pyridin-pyraxolone

Density, gravimetric

Fluoride, calorimetric, zirconium-eriochrome cyanine R

Fluoride, electrometric, ion-selective electrode

Fluoride, electrometric, ion-selective electrode, automated-segmented flow

Fluoride, ion-exchange chromatographic, automated

Hardness, calculation

Hardness, titrimetric, complexometric

Hardness, noncarbonate. calculation

Iodide, calorimetric, ceric-arsenious oxidation

Iodide, calorimetric, cerioarsenious oxidation, automated-segmented flow

Iodide, titrimetric, bromine oxidation

Iron, atomic absorption spectrometric, direct

Iron, atomic emission spectrometric, ICP

Iron, total-in-sediment, atomic absorption spectrometric, direct

Lead, atomic absorption spectrometric, chelation-extraction

Lead, atomic absorption spectrometric, direct

Lead, atomic absorption spectrometric, graphite furnace

Lead, atomic emission spectrometric, ICP

Lead, total-in-sediment, atomic absorption spectrometric, direct

Lithium, atomic absorption spectrometric, direct

Lithium, atomic emission spectrometric, ICP

Lithium, total-in sediment, atomic absorption spectrometric

Magnesium, atomic absorption spectrometric, direct

Magnesium, atomic absorption spectrometric, direct-EPA

Magnesium, atomic emission spectrometric, ICP

Magnesium, total-in-sediment, atomic absorption spectrometric, direct

Manganese, atomic absorption spectrometric, chelation-extraction

Manganese, atomic absorption spectrometric, direct

Manganese, atomic absorption spectrometric, graphite furnace

Manganese, atomic emission spectrometric, ICP

Manganese, total-in-sediment. atomic absorption spectrometric

Mercury, atomic absorption spectrometric, flameless

Mercury, atomic absorption spectrometric, flameless automated-sequential

Molybdenum, atomic absorption spectrometric, chelation-extraction

Molybdenum, atomic emission spectrometric ICP

Nickel, atomic absorption spectrometric, chelation-extraction

Nickel, atomic absorption spectrometric, direct

Nickel, atomic absorption spectrometric, graphite furnace

Nickel, total-in-sediment, atomic absorption spectrometric, direct

Nitrogen, titrimetric, digestion-distillation

Nitrogen, ammonia, colorimetric, distillation-nesslerization

Nitrogen, ammonia, colorimetric. salicylate hypochlorite automated-segmented flow

Nitrogen, ammonia, colorimetric, salicylate-hypochlorite automated-discrete

Nitrogen, ammonia, colorimetric, indophenol, automated-segmented flow

Nitrogen, ammonia, electrometric, ion-selective electrode

Nitrogen, ammonia plus organic, calorimetric, block digestor-salicylate-hypochlorite, automated-segmented flow ---------------

Nitrogen, ammonia plus organic, calorimetric, block digestor-salicylate-hypochlorite, automated

Nitrogen, ammonia plus organic, calorimetric, digestion-distillation-nesslerisation

Nitrogen, ammonia plus organic, titrimetric, digestion distillation

Nitrogen, nitrate, ion-exchange chromatographic, automated

Nitrogen, nitrite, calorimetric, diaxotization

Nitrogen, nitrite, calorimetric, diaxotization, automated-segmented flow

Nitrogen, nitrite, calorimetric, diasotization, automated-discrete

Nitrogen, nitrite, ion-exchange chromatographic, automated

Nitrogen, nitrite plus nitrate, calorimetric, cadmium reduction-diaxotization, automated-segmented flow ------------- ----- -------

Nitrogen, nitrite plus nitrate, calorimetric, hydrasine reductiondiazotisation, automated-discrete

Oxygen demand, chemical (COD), calorimetric, dichromate oxidation

Oxygen demand, chemical (COD), titrimetric, dichromate oxidation

pH, electrometric, glass-electrode

Phosphorus, calorimetric, phosphomolybdate

Phosphorus, calorimetric, phosphomolybdate, automated-segmented flow

Phosphorus, calorimetric, phosphomolybdate, automated-discrete

Phosphorus, orthophosphate plus hydrolyzable, colorimetric, phosphomolybdate

Phosphorus, orthophosphate plus hydrolyzable, colorimetric, phosphomolybdate, automated-segmented flow

Phosphorus, orthophosphate, calorimetric, phosphomolybdate

Phosphorus, orthophosphate, calorimetric, phosphomolybdate, automated-segmented flow

Phosphorus, orthophosphate, calorimetric, phosphomolybdate, automated-discrete

Phosphorus, orthophosphate. ion-exchange chromatographic, automated

Phosphorus, hydrolyzable and organic, calculation

Potassium, atomic absorption spectrometric, direct

Potassium, atomic absorption spectrometric, direct-EPA

Potassium, total-in-sediment, atomic absorption spectrometric, direct

Selenium, atomic absorption spectrometric, hydride

Selenium, atomic absorption spectrometric, hydride, automated

Selenium, total-in-sediment, atomic absorption spectormetric, hydride

Silica, atomic absorption spectrometric, direct

Silica, atomic emission spectrometric, ICP

Silica, calorimetric, molybdate blue

Silica, calorimetric, molybdate blue, automated segmented flow

Silica, total-in-sediment, atomic absorption spectrometric, direct

Silver, atomic absorption spectrometric, chelation-extraction

Sodium, atomic absorption spectrometric, direct

Sodium, atomic absorption spectrometric, direct EPA

Sodium, atomic emission spectrometric, ICP

Sodium, total-in-sediment, atomic absorption spectrometric, direct

Sodium absorption ratio, calculation

Sodium, percent, calculation

Solids, residue on evaporation at 180 “C, dissolved, gravimetric

Solids, residue on evaporation at 105 “C, dissolved, gravimetric

Solids, residue on evaporation at 105 "C, total, gravimetric

Solids, residue at 106 “C, suspended, gravimetric

Solids, volatile-on-ignition, dissolved, gravimetric

Solids, volatile-on-ignition, total, gravimetric

Solids, volatile-on-ignition, suspended, gravimetric

Solids, volatile-on-ignition, total-in-bottom-material, gravimetric

Solids, nonvolatileon-ignition, dissolved, calculation

Solids, nonvolatileon-ignition, total, calculation

Solids, nonvolatile-on-ignition, suspended. calculation

Solids, sum of constituents, calculation

Specific conductance, electrometric, Wheastone bridge

Strontium, atomic absorption spectrometric, direct

Strontium, atomic emission spectrometric, ICP

Strontium, total-in-sediment, atomic absorption spectrometric, direct

Sulfate, dissolved, calorimetric, complexometric, methyl-thymol blue, automated-segmented flow

Sulfate, turbidhnetric. barium sulfate, automated-discrete

Sulfate, ion-exchange chromatographic, automated

Sulfate, titrimetric, thorin

Sulfide, titrimetric, iodometric

Thallium, atomic absorption, spectrometric, graphite furnace

Tin, atomic absorption spectrometric, hydride, automated

Titanium, total-in-sediment, atomic absorption spectrometric, direct

Turbidity, nephelometric

Vanadium, calorimetric, catalytic oxidation

Vanadium, calorimetric, catalytic oxidation, automated-segmented flow

Vanadium, atomic emission spectrometric, ICP

Zinc, atomic absorption spectrometric, direct

Zinc, atomic absorption spectrometric, graphite furnace

Zinc, atomic emission spectrometric. ICP

Zinc, total-in-sediment, atomic absorption spectrometric, direct

Metals, atomic emission spectrometric, ICP

Anions, ion-exchange chromatographic. automated

Anions, ion-exchsnge chromatographic, low ionic-strength water, automated

Metals, major, total-in-sediment, atomic absorption spectrometric, direct

Metals, major and minor, total-in-sediment, atomic absorption spectrometric, direct

Metals, minor, total-in-sediment, atomic absorption spectrometric, hydride

 


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