Standard Methods for the Examination of Water and Wastewater
© Copyright 1999 by American Public Health Association, American Water Works Association, Water Environment Federation
Part 4000 INORGANIC NONMETALLIC CONSTITUENTS
4010 INTRODUCTION
The analytical methods included in this part make use of classical wet chemical techniquesand their automated variations and such modern instrumental techniques as ion chromatography.Methods that measure various forms of chlorine, nitrogen, and phosphorus are presented. Theprocedures are intended for use in the assessment and control of receiving water quality, thetreatment and supply of potable water, and the measurement of operation and process efficiencyin wastewater treatment. The methods also are appropriate and applicable in evaluation of environmental water-quality concerns. The introduction to each procedure contains reference tospecial field sampling conditions, appropriate sample containers, proper procedures for samplingand storage, and the applicability of the method.
4020 QUALITY ASSURANCE/QUALITY CONTROL4020 A. Introduction
Without quality control results there is no confidence in analytical results reported fromtests. As described in Part 1000 and Section 3020, essential quality control measurementsinclude: method calibration, standardization of reagents, assessment of individual capability toperform the analysis, performance of blind check samples, determination of the sensitivity of thetest procedure (method detection level), and daily evaluation of bias, precision, and the presenceof laboratory contamination or other analytical interference. Details of these procedures,expected ranges of results, and frequency of performance should be formalized in a writtenQuality Assurance Manual and Standard Operating Procedures.For a number of the procedures contained in Part 4000, the traditional determination of biasusing a known addition to either a sample or a blank, is not possible. Examples of theseprocedures include pH, dissolved oxygen, residual chlorine, and carbon dioxide. The inability toperform a reliable known addition does not relieve the analyst of the responsibility for evaluatingtest bias. Analysts are encouraged to purchase certified ready-made solutions of known levels of these constituents as a means of measuring bias. In any situation, evaluate precision throughanalysis of sample duplicates.Participate in a regular program (at a minimum, annually, and preferably semi-annually) of proficiency testing (PT)/performance evaluation (PE) studies. The information and analyticalconfidence gained in the routine performance of the studies more than offset any costs associated
Standard Methods for the Examination of Water and Wastewater
© Copyright 1999 by American Public Health Association, American Water Works Association, Water Environment Federation
with these studies. An unacceptable result on a PT study sample is often the first indication that atest protocol is not being followed successfully. Investigate circumstances fully to find the cause.Within many jurisdictions, participation in PT studies is a required part of laboratorycertification.Many of the methods contained in Part 4000 include specific quality-control procedures.These are considered to be the minimum quality controls necessary to successful performance of the method. Additional quality control procedures can and should be used. Section 4020Bdescribes a number of QC procedures that are applicable to many of the methods.
4020 B. Quality Control Practices
1. Initial Quality Control
See Section 3020B.1.
2. Calibration
See Section 3020B.2. Most methods for inorganic nonmetals do not have wide dynamicranges. Standards for initial calibration therefore should be spaced more closely than one orderof magnitude under these circumstances. Verify calibration by analyzing a midpoint or lowercalibration standard and blank as directed. Alternatively, verify calibration with two standards,one near the low end and one near the high end, if the blank is used to zero the instrument.
3. Batch Quality Control
See Section 3020B.3
a
through
d
.
4110 DETERMINATION OF ANIONS BY ION CHROMATOGRAPHY*#(1)4110 A. Introduction
Because of rapid changes in technology, this section is currently undergoing substantialrevision.Determination of the common anions such as bromide, chloride, fluoride, nitrate, nitrite,phosphate, and sulfate often is desirable to characterize a water and/or to assess the need forspecific treatment. Although conventional colorimetric, electrometric, or titrimetric methods areavailable for determining individual anions, only ion chromatography provides a singleinstrumental technique that may be used for their rapid, sequential measurement. Ionchromatography eliminates the need to use hazardous reagents and it effectively distinguishesamong the halides (Br
–
, Cl
–
, and F
–
) and the oxy-ions (SO
32–
, SO
42–
or NO
2–
, NO
3–
).This method is applicable, after filtration to remove particles larger than 0.2
µ
m, to surface,
Standard Methods for the Examination of Water and Wastewater
© Copyright 1999 by American Public Health Association, American Water Works Association, Water Environment Federation
ground, and wastewaters as well as drinking water. Some industrial process waters, such asboiler water and cooling water, also may be analyzed by this method.
4110 B. Ion Chromatography with Chemical Suppression of EluentConductivity
1. General Discussion
a. Principle:
A water sample is injected into a stream of carbonate-bicarbonate eluent andpassed through a series of ion exchangers. The anions of interest are separated on the basis of their relative affinities for a low capacity, strongly basic anion exchanger (guard and separatorcolumns). The separated anions are directed through a hollow fiber cation exchanger membrane(fiber suppressor) or micromembrane suppressor bathed in continuously flowing strongly acidsolution (regenerant solution). In the suppressor the separated anions are converted to theirhighly conductive acid forms and the carbonate-bicarbonate eluent is converted to weaklyconductive carbonic acid. The separated anions in their acid forms are measured by conductivity.They are identified on the basis of retention time as compared to standards. Quantitation is bymeasurement of peak area or peak height.
b. Interferences:
Any substance that has a retention time coinciding with that of any anion tobe determined and produces a detector response will interfere. For example, relatively highconcentrations of low-molecular-weight organic acids interfere with the determination of chloride and fluoride by isocratic analyses. A high concentration of any one ion also interfereswith the resolution, and sometimes retention, of others. Sample dilution or gradient elutionovercomes many interferences. To resolve uncertainties of identification or quantitation use themethod of known additions. Spurious peaks may result from contaminants in reagent water,glassware, or sample processing apparatus. Because small sample volumes are used,scrupulously avoid contamination. Modifications such as preconcentration of samples, gradientelution, or reinjection of portions of the eluted sample may alleviate some interferences butrequire individual validation for precision and bias.
c. Minimum detectable concentration:
The minimum detectable concentration of an anion isa function of sample size and conductivity scale used. Generally, minimum detectableconcentrations are near 0.1 mg/L for Br
–
, Cl
–
, NO
3–
, NO
2–
, PO
43–
, and SO
42–
with a 100-
µ
Lsample loop and a 10-
µ
S/cm full-scale setting on the conductivity detector. Lower values may beachieved by using a higher scale setting, an electronic integrator, or a larger sample size.
d. Limitations:
This method is not recommended for the determination of F
–
in unknownmatrices. Equivalency studies have indicated positive or negative bias and poor precision insome samples. Recent interlaboratory studies show acceptable results. Two effects are common:first, F
–
is difficult to quantitate at low concentrations because of the major negative contributionof the ‘‘water dip’’ (corresponding to the elution of water); second, the simple organic acids(formic, carbonic, etc.) elute close to fluoride and will interfere. Determine precision and bias
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