NITROGEN (4500-N)/Introduction 4-103

4500-N NITROGEN*

4500-N A. Introduction

In waters and wastewaters the forms of nitrogen of greatest oxidation and reduction may occur in wastewater treatment plants,
interest are, in order of decreasing oxidation state, nitrate, nitrite, water distribution systems, and natural waters. Nitrite can enter a
ammonia, and organic nitrogen. All these forms of nitrogen, as water supply system through its use as a corrosion inhibitor in
well as nitrogen gas (N2), are biochemically interconvertible and industrial process water. Nitrite is the actual etiologic agent of
are components of the nitrogen cycle. They are of interest for methemoglobinemia. Nitrous acid, which is formed from nitrite in
many reasons. acidic solution, can react with secondary amines (RR⬘NH) to form
Organic nitrogen is defined functionally as organically bound nitrosamines (RR⬘N-NO), many of which are known to be carcin-
nitrogen in the trinegative oxidation state. It does not include all ogens. The toxicologic significance of nitrosation reactions in vivo
organic nitrogen compounds. Analytically, organic nitrogen and and in the natural environment is the subject of much current
ammonia can be determined together and have been referred to concern and research.
as “kjeldahl nitrogen,” a term that reflects the technique used in Ammonia is present naturally in surface and wastewaters. Its
their determination. Organic nitrogen includes such natural ma-
concentration generally is low in groundwaters because it ad-
terials as proteins and peptides, nucleic acids and urea, and
sorbs to soil particles and clays and is not leached readily from
numerous synthetic organic materials. Typical organic nitrogen
soils. It is produced largely by deamination of organic nitrogen-
concentrations vary from a few hundred micrograms per liter in
some lakes to more than 20 mg/L in raw sewage. containing compounds and by hydrolysis of urea. At some water
Total oxidized nitrogen is the sum of nitrate and nitrite nitro- treatment plants ammonia is added to react with chlorine to form
gen. Nitrate generally occurs in trace quantities in surface water a combined chlorine residual. Ammonia concentrations encoun-
but may attain high levels in some groundwater. In excessive tered in water vary from less than 10 ␮g ammonia nitrogen/L in
amounts, it contributes to the illness known as methemoglobin- some natural surface and groundwaters to more than 30 mg/L in
emia in infants. A limit of 10 mg nitrate as nitrogen/L has been some wastewaters.
imposed on drinking water to prevent this disorder. Nitrate is In this manual, organic nitrogen is referred to and reported as
found only in small amounts in fresh domestic wastewater but in organic N, nitrate nitrogen as NO3⫺-N, nitrite nitrogen as
the effluent of nitrifying biological treatment plants nitrate may NO2⫺-N, and ammonia nitrogen as NH3-N.
be found in concentrations of up to 30 mg nitrate as nitrogen/ L. Total nitrogen can be determined through oxidative digestion
It is an essential nutrient for many photosynthetic autotrophs and of all digestible nitrogen forms to nitrate, followed by quantita-
in some cases has been identified as the growth-limiting nutrient. tion of the nitrate. Two procedures, one using a persulfate/UV
Nitrite is an intermediate oxidation state of nitrogen, both in the digestion (4500-N.B), and the other using persulfate digestion
oxidation of ammonia to nitrate and in the reduction of nitrate. Such (4500-N.C) are presented. The procedures give good results for
total nitrogen, composed of organic nitrogen (including some
aromatic nitrogen-containing compounds), ammonia, nitrite, and
* Approved by Standard Methods Committee, A,B,C, 1997; D, 2001.
Joint Task Group: (4500-N. D)—Thomas R. Holm (chair); 20th Edition (4500-N. nitrate. Molecular nitrogen is not determined and recovery of
B)—Scott Stieg (chair), Bradford R. Fisher, Owen B. Mathre, Theresa M. Wright. some industrial nitrogen-containing compounds is low.
4-104 INORGANIC NONMETALS (4000)

Chloride ions do not interfere with persulfate oxidation, but are obtained; if it is not dissolved, the results are unreliable and
the rate of reduction of nitrate to nitrite (during subsequent probably reflect a negative interference. The persulfate method is
nitrate analysis by cadmium reduction) is significantly decreased not effective in wastes with high organic loadings. Dilute such
by chlorides. Ammonium and nitrate ions adsorbed on sus- samples and re-analyze until results from two dilutions agree.
pended pure clay or silt particles should give a quantitative yield A conductimetric method (4500-N.D) for the determination of
from persulfate digestion. If suspended matter remains after inorganic nitrogen also is presented.
digestion, remove it before the reduction step.
If suspended organic matter is dissolved by the persulfate
digestion reagent, yields comparable to those from true solutions

4500-N B. In-Line UV/Persulfate Digestion and Oxidation with Flow Injection Analysis

1. General Discussion

a. Principle: Nitrogen compounds are digested and oxi-

dized in-line to nitrate by use of heated alkaline persulfate and
ultraviolet radiation. The digested sample is injected onto the
manifold where its nitrate is reduced to nitrite by a cadmium
granule column. The nitrite then is determined by diazotiza-
tion with sulfanilamide under acidic conditions to form a
diazonium ion. The diazonium ion is coupled with N-(1-
naphthyl)ethylenediamine dihydrochloride. The resulting
pink dye absorbs at 540 nm and is proportional to total
nitrogen.
This method recovers nearly all forms of organic and inor-
ganic nitrogen, reduced and oxidized, including ammonia, ni-
trate, and nitrite. It differs from the total kjeldahl nitrogen
Figure 4500-N:1. FIA in-line total nitrogen manifold.
method described in Section 4500-Norg.D, which does not re-
cover the oxidized forms of nitrogen. This method recovers
nitrogen components of biological origin such as amino acids,
proteins, and peptides as ammonia, but may not recover the
nitrogenous compounds of some industrial wastes such as proportionally. Use manifold tubing of an inert material such as
amines, nitro-compounds, hydrazones, oximes, semicarbazones, TFE. The block marked “UV” should consist of TFE tubing
and some refractory tertiary amines. irradiated by a mercury discharge ultraviolet lamp emitting ra-
See Section 4500-N.A for a discussion of the various forms of diation at 254 nm.
nitrogen found in waters and wastewaters, Sections 4500-Norg.A d. Absorbance detector, 540 nm, 10-nm bandpass.
and B for a discussion of total nitrogen methods, and Section e. Injection valve control and data acquisition system.
4130, Flow Injection Analysis (FIA). Also see Section 4500-N.C
for a similar, batch total nitrogen method that uses only persul- 3. Reagents
fate.
b. Interferences: Remove large or fibrous particulates by fil- Use reagent water (⬎10 megohm) to prepare carrier and for all
tering sample though glass wool. Guard against contamination solutions. To prevent bubble formation, degas carrier and all
from reagents, water, glassware, and the sample preservation reagents with helium. Pass He at 140 kPa (20 psi) through a
process. helium degassing tube. Bubble He through 1 L solution for 1
min. As an alternative to preparing reagents by weight/weight,
2. Apparatus use weight/volume.
a. Borate solution, Na2B4O7 䡠 10H2O: In a 1-L volumetric
Flow injection analysis equipment consisting of: flask dissolve 38.0 g Na2B4O7 䡠 10H2O and 3.0 g sodium hy-
a. FIA injection valve with sample loop or equivalent. droxide, NaOH, in approximately 900 mL water, using a mag-
b. Multichannel proportioning pump. netic stirring bar. Gentle heating will speed dissolution. Adjust to
c. FIA manifold (Figure 4500-N:1) with tubing heater, in-line pH 9.0 with NaOH or conc hydrochloric acid (HCl). Dilute to
ultraviolet digestion fluidics including a debubbler consisting of mark and invert to mix.
a gas-permeable TFE membrane and its holder, and flow cell. In b. Persulfate solution, K2S2O8: Potassium persulfate solid
Figure 4500-N:1, relative flow rates only are shown. Tubing reagent usually contains nitrogen contamination. Higher contam-
volumes are given as an example only; they may be scaled down ination levels result in larger blank peaks.
NITROGEN (4500-N)/Persulfate Method 4-105

To a tared 1-L container, add 975 g water and 49 g K2S2O8. TABLE 4500-N:I. RECOVERIES OF TOTAL NITROGEN
Add a magnetic stirring bar, dissolve persulfate, and dilute to
Mean Recovery
mark. Invert to mix. %
c. Ammonium chloride buffer: CAUTION: Fumes. Use a hood.
Compound 10 mg N/L 4 mg N/L
To a 1-L volumetric flask add 500 mL water, 105 mL conc HCl,
and 95 mL conc ammonium hydroxide, NH4OH. Dissolve, dilute Ammonium chloride 98.1 99.7
to mark, and invert to mix. Adjust to pH 8.5 with 1N HCl or 1N Sodium nitrite 100.5 101.8
NaOH solution. Glycine 101.0 100.8
d. Sulfanilamide color reagent: To a tared, dark, 1-L con- Glutamic acid 99.7 99.2
tainer add 876 g water, 170 g 85% phosphoric acid, H3PO4, Ammonium p-toluenesulfonate 99.6 97.4
Glycine p-toluenesulfonate 101.4 102.3
40.0 g sulfanilamide, and 1.0 g N-(1-naphthyl)ethylenediamine
Nicotinic acid 98.6 102.0
dihydrochloride (NED). Shake to wet solids and stir for 30 min Urea 94.9 98.0
to dissolve. Store in a dark bottle and discard when solution turns EDTA 89.4 89.4
dark pink.
e. Cadmium column: See Section 4500-NO3⫺.I.3c, d, and e.
f. Stock nitrate standard, 1000 mg N/L: In a 1-L volumetric
6. Quality Control
flask dissolve 7.221 g potassium nitrate, KNO3 (dried at 60°C for
1 h), or 4.93 g sodium nitrite, NaNO2, in about 800 mL water.
See Section 4130B.
Dilute to mark and invert to mix. When refrigerated the standard
may be stored for up to 3 months.
7. Precision and Bias
g. Standard solutions: Prepare nitrate standards in the desired
concentration range, using stock nitrate standards (¶ 3f), and
a. MDL: Using a 70-␮L sample loop and a published MDL
diluting with water.
method,1 analysts ran 21 replicates of a 0.20-mg N/L standard.
These gave a mean of 0.18 mg N/L, a standard deviation of 0.008
4. Procedure
mg N/L, and MDL of 0.020 mg N/L.
b. Precision study: Ten injections each of a 4.00-mg N/L
Set up a manifold equivalent to that in Figure 4500-N:1 and standard and of a 10.0-mg N/L standard both gave a relative
follow method supplied by manufacturer, or laboratory standard standard deviation of 0.6%.
operating procedure for this method. c. Recovery of total nitrogen: Table 4500-N:I shows recov-
Carry both standards and samples through this procedure. If eries for various nitrogen compounds determined at 10 mg N/L
samples have been preserved with sulfuric acid, preserve stan- and 4.0 mg N/L. All compounds were determined in triplicate.
dards similarly. Samples may be homogenized. Turbid samples d. Ammonia recoveries from wastewater treatment plant ef-
may be filtered, since digestion effectiveness on nitrogen-con- fluent with known additions: To a sample of wastewater treat-
taining particles is unknown; however, organic nitrogen may be ment plant effluent, ammonium chloride was added at two con-
lost in the filtration. centrations, 2.50 and 5.00 mg N/L, and analyses were made in
triplicate to give mean recoveries of 96% and 95%, respectively.
5. Calculation A sample with no additions also was diluted twofold in triplicate
to give a mean recovery of 99%.
Prepare standard curves by plotting absorbance of standards
processed through the manifold versus nitrogen concentration. 8. Reference
The calibration curve is linear.
Verify digestion efficiency by determining urea, glutamic 1. U.S. ENVIRONMENTAL PROTECTION AGENCY. 1984. Definition and pro-
acid, or nicotinic acid standards (4500-N.C.3d) at regular inter- cedure for the determination of method detection limits. Appendix B
vals. In the concentration range of the method, the recovery of to 40 CFR 136 Rev. 1.11 amended June 30, 1986. 49 CFR 43430,
these compounds should be ⬎95%. October 26, 1984.

4500-N C. Persulfate Method

1. General Discussion a. Principle: Alkaline oxidation at 100 to 110°C converts

organic and inorganic nitrogen to nitrate. Total nitrogen is de-
The persulfate method determines total nitrogen by oxidation termined by analyzing the nitrate in the digestate.
of all nitrogenous compounds to nitrate. Should ammonia, ni- b. Selection of nitrate measurement method: Automated or
trate, and nitrite be determined individually, “organic nitrogen” manual cadmium reduction may be used to determine total
can be obtained by difference. nitrogen levels below 2.9 mg N/L. Results summarized in Table
4500-N:II were obtained using automated cadmium reduction.
4-106 INORGANIC NONMETALS (4000)

TABLE 4500-N:II. PRECISION DATA FOR TOTAL NITROGEN, f. Digestion reagent: Dissolve 20.1 g low nitrogen (⬍0.001%
PERSULFATE METHOD, BASED ON TRIPLICATE ANALYSES OF N) potassium persulfate, K2S2O8, and 3.0 g NaOH in water and
NICOTINIC ACID dilute to 1000 mL just before use.
Relative g. Borate buffer solution: Dissolve 61.8 g boric acid, H3BO3,
Nicotinic Recovery of Standard Standard and 8.0 g NaOH in water and dilute to 1000 mL.
Lab/ Acid N Deviation Deviation h. Copper sulfate solution: Dissolve 2.0 g CuSO4 䡠 5H2O in
Analyst mg N/L % mg/L % 90 mL water and dilute to 100 mL.
i. Ammonium chloride solution: Dissolve 10.0 g NH4Cl in 1 L
1/1 0.5 104 0.019 3.82
water. Adjust to pH 8.5 by adding three or four NaOH pellets as
1/2 0.5 99.7 0.012 2.44
2/1 0.5 97.7 0.035 7.02 necessary or NaOH solution before bringing to volume. This
2/2 0.5 87.8 0.024 4.89 reagent is stable for 2 weeks when refrigerated.
3/1 0.5 105 0.072 13.7 j. Color reagent: Combine 1500 mL water, 200.0 mL conc
3/2 0.5 95.3 0.015 3.20 phosphoric acid, H3PO4, 20.0 g sulfanilamide, and 1.0 g N-(1-
1/1 1.0 98.5 0.023 2.32 naphthyl)-ethylenediamine dihydrochloride. Dilute to 2000 mL.
1/2 1.0 99.3 0.022 2.21 Add 2.0 mL polyoxyethylene 23 lauryl ether.† Store at 4°C in
2/1 1.0 113 0.053 5.31 the dark. Prepare fresh reagent every 6 weeks. Alternatively,
2/2 1.0 97.1 0.031 3.10 prepare proportionally smaller volumes to minimize waste.
3/1 1.0 96.2 0.019 1.97
3/2 1.0 102 0.025 2.46 4. Procedure
1/1 2.0 100 0.030 1.50
1/2 2.0 97.8 0.014 0.7 a. Calibration curve: Prepare NO3⫺ calibration standards in
2/1 2.0 104 0.069 3.45 the range 0 to 2.9 mg NO3⫺-N/L by diluting to 100 mL the
2/2 2.0 100 0.080 3.98
following volumes of intermediate nitrate solution: 0, 1.00, 2.00,
3/1 2.0 95.3 0.078 4.12
3/2 2.0 98.3 0.015 0.75 4.00 . . . 29.0 mL. Treat standards in the same manner as sam-
ples.
b. Digestion check standard: Prepare glutamic acid digestion
check standard of 2.9 mg N/L by diluting, to 100 mL, a 29.0-mL
volume of intermediate glutamic acid solution. Treat digestion
2. Apparatus check standard in the same manner as samples.
c. Digestion: Samples preserved with acid cannot be analyzed
a. Autoclave, or hotplate and pressure cooker capable of by this method. To a culture tube, add 10.0 mL sample or
developing 100 to 110°C for 30 min. standard or a portion diluted to 10.0 mL. Add 5.0 mL digestion
b. Glass culture tubes:* 30-mL screw-capped (polypropylene reagent. Cap tightly. Mix by inverting twice. Heat for 30 min in
linerless caps), 20 mm OD ⫻ 150 mm long. Clean before initial an autoclave or pressure cooker at 100 to 110°C. Slowly cool to
use by autoclaving with digestion reagent. room temperature. Add 1.0 mL borate buffer solution. Mix by
c. Apparatus for nitrate determination: See Section 4500- inverting at least twice.
NO3⫺.E or F. d. Blank: Carry a reagent blank through all steps of the
d. Automated analytical equipment: An example of the con- procedure and apply necessary corrections to the results.
tinuous-flow analytical instrument consists of components e. Nitrate measurement: Determine nitrate by cadmium re-
shown in Figure 4500-NO3⫺:2. duction. Set up manifold as shown in Figure 4500-NO3⫺:2, but
use reagents specified in 4500-Norg.C.3.
3. Reagents
5. Calculation
a. Ammonia-free and nitrate-free water: Prepare by ion ex-
Prepare the standard curve by plotting the absorbances or peak
change or distillation methods as directed in 4500-NH3.B.3a and
heights of the nitrate calibration standards carried through the
4500-NO3⫺.B.3a.
digestion procedure against their nitrogen concentrations. Com-
b. Stock nitrate solution: Prepare as directed in 4500-
pute organic N sample concentration by comparing sample ab-
NO3⫺.B.3b.
sorbance or peak height with the standard curve.
c. Intermediate nitrate solution: Prepare as directed in 4500-
NO3⫺.B.3c. 6. Precision and Bias
d. Stock glutamic acid solution: Dry glutamic acid,
C3H5NH2(COOH)2, in an oven at 105°C for 24 h. Dissolve 1.051 See Table 4500-N:II.
g in water and dilute to 1000 mL; 1.00 mL ⫽ 100 ␮g N. Preserve
with 2 mL CHCl3/L. 7. Bibliography
e. Intermediate glutamic acid solution: Dilute 100 mL stock
glutamic acid solution to 1000 mL with water; 1.00 mL ⫽ 10.0 D’ELIA, C.F., P.A. STEUDLER & N. CORWIN. 1977. Determination of total
␮g N. Preserve with 2 mL CHCl3/L. nitrogen in aqueous samples using persulfate digestion. Limnol.
Oceanogr. 22:760.

*18 – 415, Comar, Inc., Vineland, NJ, or equivalent. † Brij-35, available from ICI Americas, Inc., Wilmington, DE, or equivalent.
NITROGEN (4500-N)/Conductimetric Determination of Inorganic Nitrogen 4-107

NYDAHL, F. 1978. On the peroxodisulphate oxidation of total nitrogen in AMEEL, J.J., R.P. AXLER & C.J. OWEN. 1993. Persulfate digestion for
waters to nitrate. Water Res. 12:1123. determination of total nitrogen and phosphorus in low-nutrient
VALDERRAMA, J.C. 1981. The simultaneous analysis of total nitrogen and waters. Amer. Environ. Lab. 10/93:1.
total phosphorus in natural waters. Mar. Chem. 10:109.
EBINA, J., T. TSUTSUI & T. SHIRAI. 1983. Simultaneous determination of
total nitrogen and total phosphorus in water using peroxodisulfate
oxidation. Water Res. 17:1721.

4500-N D. Conductimetric Determination of Inorganic Nitrogen

1. General Discussion reduces both nitrite and nitrate to ammonia, differentiation be-
tween the two ions is not possible with this method.
a. Principle: Aqueous ammonia nitrogen in samples is con- b. Interferences: Remove particulate matter by filtration be-
verted to dissolved ammonia gas by raising sample pH above 11 fore analysis to prevent plugging of analyzer lines.
with alkaline solution. The sample/alkaline solution is placed in Calcium and magnesium precipitate formation can clog ana-
one cell of a two-cell diffusion chamber with a buffered absorb- lyzer lines. Prevent precipitate formation by adding diethylene-
ing solution in the second cell. A hydrophobic membrane, triaminepentaacetic acid (DTPA) to the alkaline feed at a con-
through which the dissolved ammonia gas diffuses, separates the centration up to 10 g/L.
cells. The pH of the absorbing solution is neutral, facilitating Volatile amines, chloramines, or the amides of carboxylic
conversion of the dissolved ammonia gas to the ammonium ion acids can diffuse through the hydrophobic membrane to produce
form. Change in conductivity of the absorbing solution is deter- a conductivity response or react in the diffusion cell to form
mined in a conductivity cell. The method is best applied using a ammonia. Reduce or eliminate this response for volatile amines
continuous-flow conductimetric system such as shown in Figure or the amides of carboxylic acids by adjusting pH of the alkaline
4500-N:2. In the continuous-flow system, samples are injected solution below pKa of the amine or amide but above pKa of
into a continuously fed stream of alkaline solution at selected ammonia. Reduce or eliminate this response for chloramines by
time intervals, usually 1 to 2 min, and pass through the system as not reducing the chloramines over zinc to ammonia.
plugs. Response time usually is less than 1 min. c. Minimum detectable concentration: The estimated mini-
Total oxidized inorganic nitrogen (nitrate and/or nitrite) is mum detectable concentration of NH3-N or combined NO3⫺-N
measured by reducing to ammonia with zinc after mixing sample and NO2⫺-N is 0.01 mg/L.2
with the alkaline solution.1 The reaction is d. Storage of samples: Optional storage conditions for samples
depend on the forms of nitrogen and interferences present. Refer
to 4500-NH3.A.3, 4500-NO2⫺.B.1c, or 4500-NO3⫺.A.2 for spe-
NO⫺ ⫺
3 ⫹ 4Zn ⫹ 7OH 3 NH3 ⫹ 4ZnO2 ⫹ 2H2O
2⫺
cific conditions.

In the continuous-flow system, a zinc reduction cartridge is 2. Apparatus

placed in the flow stream, as indicated in Figure 4500-N:2.
The reduction reaction is catalyzed by copper; addition of Automated analytical equipment: An example of the auto-
copper sulfate to the alkaline solution is beneficial. mated, continuous-flow analytical equipment required is shown
When both ammonia and oxidized forms of nitrogen are in Figure 4500-N:2. Details of the requirements and current
present in a sample, the total nitrogen and the ammonia nitrogen manufacturers of commercial apparatus* can be found in the
concentrations are determined separately and the oxidized nitro- literature.3
gen is calculated by difference. Because the reaction with zinc
3. Reagents

Use ammonia-free, deionized water for making all reagents.

a. Ammonia standards: Prepare at least three standard ammo-
nia nitrogen standards in the desired analysis range between 0.1
and 75 mg N/L by dissolving an appropriate quantity of ammo-
nium sulfate, (NH4)2SO4, in water and diluting to 1 L.
b. Nitrate standards: Prepare at least three standard nitrate-
nitrogen standards in analysis range between 0.1 mg and 75 mg
N/L by dissolving an appropriate quantity of sodium nitrate,
NaNO3, in water and diluting to 1 L.

* Timberline Instruments, 1800 S. Flatiron Court, Boulder, CO 80301 (www.

Figure 4500-N:2. Continuous-flow conductimetric analyzer system. [Link]).
4-108 INORGANIC NONMETALS (4000)

c. Alkaline solution I (for determination of ammonia nitrogen): demonstrate method proficiency and to evaluate method bias.
Dissolve 25 g potassium hydroxide, KOH, and 10 g diethylene- Certain regulatory programs may have more extensive QC re-
triaminepentaacetic acid, DTPA, precipitate inhibitor in 1 L quirements.
water.
d. Copper catalyst solution: Dissolve 200 mg CuSO4䡠5H2O in 7. Precision and Bias
1 L water.
e. Alkaline solution II (for determination of nitrate and nitrite Ammonia standard concentrations of 0.1, 0.8, 5, 15, 30, 55,
nitrogen): Dissolve 25 g potassium hydroxide, KOH, 10 g di- and 75 mg/L NH3-N were analyzed. Recovery ranged from
ethylenetriaminepentaacetic acid, DTPA, precipitate inhibitor, 99.31 and 101.64% at concentrations of 5 and 0.1 mg/L NH3-N,
and 10 mL copper catalyst solution in 1 L water. respectively. Precision ranged from 0.33 to 3.57% for concen-
f. Absorbent solution: Dissolve 100 mg boric acid, H3BO3, in trations of 15 and 0.1 mg/L NH3-N, respectively.
1 L water. Adjust to pH 7 with ammonium hydroxide, NH4OH. Nitrate standard concentrations of 0.1, 0.8, 5, 15, 30, 55, and
g. Zinc reduction cartridges, containing 20/30 mesh zinc 75 mg/L NO3⫺-N were analyzed. Recovery ranged from 99.93 to
metal. 101.84% at concentrations of 75 and 0.8 mg/L NO3⫺-N, respec-
tively. Precision ranged from 0.64 to 4% at concentrations of 75
4. Procedure and 0.1 mg/L NO3⫺-N, respectively.
Combined nitrogen standards were prepared using 50% por-
Set up instrument equivalent to that in Figure 4500-N:2 and tions of NH3-N and NO3⫺-N. Concentrations analyzed were 0.1,
follow manufacturer’s operating procedure. Calibrate instrument 0.8, 5, 15, 30, 50, and 75 mg N/L. Ranges of recovery and
using appropriate standard solutions and insert a standard every precision of the combined nitrogen analysis were 99.83 to
tenth tube in the autosampler tray. Filter turbid samples before 101.58% and 0.45 and 4.22%. Ranges of recovery and precision
analysis. of the ammonia nitrogen analysis were 97.68 to 106.19% and
2.58 to 12.1%. Ranges of recovery and precision for the calcu-
5. Calculation lated nitrate nitrogen were 95.08 to 104.08% and 0.84 and 11%.2
8. References
Prepare standard curves by plotting nitrogen concentration of
standards versus conductivity of absorbent solution. The calibra-
1. CARLSON, R.M. 1986. Continuous flow reduction of nitrate to ammo-
tion is linear. Compute sample nitrogen concentration by com-
nia with granular zinc. Anal. Chem. 58:1590.
paring sample conductivity with standard curve. 2. MANSELL, B.O. & E.D. SCHROEDER. 2000. Automated separation and
conductimetric determination of inorganic nitrogen. J. Environ. Eng.
6. Quality Control 126:778.
3. CARLSON, R.M. 1978. Automated separation and conductimetric de-
See Section 4020 for minimum quality assurance/quality con- termination of ammonia and dissolved carbon dioxide. Anal. Chem.
trol (QA/QC) guidelines. It is the analyst’s responsibility to 50:1528.