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EPA-600/4-78-015
February 1978
600478015
Environmental Monitoring Series
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RESEARCH REPORTING SERIES
Research reports of the Office of Research and Development, U.S. Environmental
Protection Agency, have been grouped into nine series. These nine broad cate-
gories were established to facilitate further development and application of en-
vironmental technology. Elimination of traditional grouping was consciously
planned to foster technology transfer and a maximum interface in related fields.
The nine series are:
1. Environmental Health Effects Research
2. Environmental Protection Technology
3. Ecological Research
4. Environmental Monitoring
5. Socioeconomic Environmental Studies
6. Scientific and Technical Assessment Reports (STAR)
7. Interagency Energy-Environment Research and Development
8. "Special" Reports
9. Miscellaneous Reports
This report has been assigned to the ENVIRONMENTAL MONITORING series.
This series describes research conducted to develop new or improved methods
and instrumentation for the identification and quantification of environmental
pollutants at the lowest conceivably significant concentrations. It also includes
studies to determine the ambient concentrations of pollutants in the environment
and/or the variance of pollutants as a function of time or meteorological factors.
This document is available to the public through the National Technical Informa-
tion Service, Springfield, Virginia 22161.
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EPA-600/4-78-015
February 1978
EVALUATION OF THE TECHNICON BLOCK DIGESTOR SYSTEM
'FOR TOTAL KJELDAHL NITROGEN AND TOTAL PHOSPHORUS
by
Morris E. Gales, Jr.
Physical and Chemical Methods Branch
Environmental Monitoring and Support Laboratory
Cincinnati, Ohio 45268
Robert L. Booth
Office of the Director
Environmental Monitoring and Support Laboratory
Cincinnati, Ohio 45268
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
U.S. ENVIRONMENTAL PROTECTION AGENCY
CINCINNATI, OHIO 45268
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DISCLAIMER
This report has been reviewed by the Environmental Monitoring and
Support Laboratory, U. S. Environmental Protection Agency, and approved for
publication. Mention of trade names or commercial products does not consti-
tute endorsement or recommendation for use.
11
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FOREWORD
Environmental measurements are required to determine the quality of
ambient waters and the character of waste effluents. The Environmental
Monitoring and Support Laboratory - Cincinnati conducts research to:
o Develop and evaluate techniques to measure the presence and
concentration of physical, chemical, and radiological pollutants
in water, wastewater, bottom sediments, and solid waste.
o Investigate methods for the concentration, recovery, and
identification of viruses, bacteria, and other microbiological
organisms in water. Conduct studies to determine the responses
of aquatic organisms to water quality.
o Conduct an Agency-wide quality assurance program to assure
standardization and quality control of systems for monitoring
water and wastewater.
There is an ever-increasing interest in the use of automated methods
to analyze water and waste samples, whether the resulting data are to be
used for research, surveillance, compliance monitoring, or enforcement
purposes. Accordingly, the Environmental Monitoring and Support Laboratory
has an on-going methods research effort in the development, evaluation, and
modification of automated colorimetric procedures. This particular report
pertains to the simultaneous and semi-automated determination of two key
nutrient parameters: total phosphorus and total Kjeldahl nitrogen. The
method has potential routine application for the analysis of these constitu-
ents in drinking waters, surface water, and domestic and industrial wastes.
Dwight G. Ballinger
Director
Environmental Monitoring and Support Laboratory - Cincinnati
111
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ABSTRACT
Technicon's block digester method for the simultaneous determination of
total phosphorus and total Kjeldahl nitrogen has been evaluated and modified
for the semi-automated determination of these constituents in surface water
and domestic and industrial wastes. The Technicon digestion mixture was
replaced with the Kjeldahl nitrogen digestion solution. The applicable
range is 0.1 to 20 mg per liter for phosphorus and nitrogen.
IV
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• CONTENTS
Page
Foreword iii
Abstract iv
List of Tables vi
Section I - Introduction 1
Section II - Conclusion 2
Section III - Experimental Procedures 3
Section IV - Data 6
Section V - References 9
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LIST OF TABLES
Number Page
1 Concentration Ranges (Nitrogen) 10
2 Recovery of Nitrogen from Cysteine and Nicotinic
Acid with the Block Digester System 11
3 Recovery of Phosphorus and Nitrogen from
Adenosine-5-Phosphate with the Block Digester System 11
4 Comparison of Technicon's System and the Modified System 12
5 Comparison of TKN Data Obtained for Nicotinic Acid Using
the 1 X 8" and 1 X 10" Digestion Tubes 12
6 Recovery of Ammonia from Ammonium Chloride and QAL
Reference Sample 12
7 Recovery of Nitrogen and Phosphorus from Sewage Samples 13
8* Recovery of Nitrogen and Phosphorus from Organic Compounds
added to Ohio River Water 13
9 Comparison of Nitrogen Results, Colorimetric Method vs.
the Ammonia Probe, mg N/l 14
VI
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SECTION I
INTRODUCTION
Organic nitrogen and phosphorus have been considered important water
quality parameters because of their association with human and industrial
waste. Before these parameters can be analyzed, samples have to be digested.
For analysis of phosphorus the sample is digested using sulfuric acid and
persulfate (1) to convert all the phosphorus to orthophosphate. The Kjeldahl
nitrogen method (1) is used for the determination of organic nitrogen. This
method converts nitrogen components of biological origin to ammonia and may
or may not be applicable for industrial wastes. An automated vanadium method
(2) was developed by the Environmental Monitoring and Support Laboratory
(EMSL) for simultaneous determination of organic nitrogen and phosphorus
in surface water and industrial wastes; however, the use of this method was
discontinued because of the hazard involved with using perchloric acid as
the oxidant. The National Pollution Discharge Elimination System (NPDES)
has increased the need for a method to replace this automated method. Tech-
nicon has developed another system, the Block Digester , that can be used to
determine organic nitrogen and phosphorus for the same sample.
The objective of this study was to evaluate the Technicon Block Digester
(BD) system (3) and determine its applicability to water and waste analyses.
This system consists of a block digestor that holds 40 digestion tubes and an
AutoAnalyzer for subsequent colorimetric analysis. Technicon's method can be
used to determine organic nitrogen and phosphorus over a range of 0.1 to 20
mg per liter in water and wastewaters at a rate of 20 to 30 samples per hour.
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SECTION II
CONCLUSION
The digestion system employed is similar to one used by two other EPA
laboratories where less sample is taken; however, the same ratio of sample
to digestion solution is maintained. The data obtained by the three lab-
oratories have shown that this system can be used to analyze surface water,
drinking water, and domestic and industrial wastes. The recovery of 73%
nitrogen from nicotinic acid shows that this system has the potential of
giving higher results than the conventional manual TKN method.
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SECTION III
EXPERIMENTAL PROCEDURES
APPARATUS
Technicon Block Digester* - BD-40
1 x 10" or 1 x 8" Pyrex digestion tubes**
Chemware TFE (Teflon) boiling stones (Markson Science Inc., Box 767,
Delmar, CA 92014)
Technicon Manifold No. 325-74W for Ammonia
Technicon Manifold No. 327-74W for Phosphorus
REAGENTS
For Digestion
Mercuric sulfate solution: Dissolve 8 g red, mercuric oxide (HgO) in
50 ml of 1:5 sulfuric acid (10.0 ml cone. F^SO^ 40 ml distilled water) and
dilute to 100 ml with distilled water.
Digestion solution (Sulfuric acid-mercuric sulfate-potassium sulfate
solution): Dissolve 133 g of ^804 in 700 ml of distilled water and 200 ml
of cone. H2S04. Add 25 ml of mercuric sulfate solution and dilute to
1 liter.
For Ammonia
Sulfuric acid solution, 4%: Add 40 ml of cone, sulfuric acid to 800 ml
of ammonia-free distilled water; cool and dilute to 1 liter.
Stock sodium hydroxide, 20%: Dissolve 200 g sodium hydroxide in about
800 ml of ammonia-free water and dilute to 1 liter.
Stock sodium potassium tartrate solution, 20%: Dissolve 200 g sodium
potassium tartrate in about 800 ml of ammonia-free distilled water and
dilute to 1 liter.
Stock buffer solution: Dissolve 134 g of sodium phosphate, dibasic
(Na2HPO.), in about 300 ml of ammonia-free water. Add 20 g of sodium hy-
droxide and dilute to 1 liter.
* The Environmental Research Center, Corvallis, OR has also developed a
block digestion system that can be used on a hot plate.
**If the 8" tubes are used, two inches have to be cut off of the bottom of
the tube rack.
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Working buffer solution: Combine the reagents in the stated order;
add 250 ml of stock sodium potassium tartrate solution to 200 ml of stock
buffer solution and mix. Add ml amounts *** sodium hydroxide solution and
dilute to 1 liter. The pH of this solution should be above 12.9.
Sodium salicylate/sodium nitroprusside solution: Dissolve 150 g of
sodium salicylate and 0.3 g of sodium nitroprusside in about 600 ml of
ammonia free water and dilute to 1 liter.
Sodium hypochlorite solution: Dilute 6.0 ml of sodium hypochlorite
solution to 100 ml with ammonia-free distilled water.
Stock standard solution: In distilled water, dissolve 3.819 g of anhy-
drous ammonium chloride (NH.C1) dried at 105°C, and dilute to 1000 ml.
1.0 mg = 1.0 mg NH3-N.
For Phosphorus
Sulfuric acid solution, 0.72 N: Add 10 ml of cone, sulfuric acid to
300 ml of distilled water, mix, and dilute to 500 ml.
Molybdate/Antimoiiy Solution: Dissolve 8 g of ammonium molybdate and
0.2 g of antimony potassium tartrate in about 800 ml of distilled water and
dilute to 1 liter.
Ascorbic Acid Solution: Dissolve 60 g of ascorbic acid in about 600 ml
of distilled water. Add 2 ml of acetone and dilute to 1 liter.
Sodium chloride solution: Dissolve 40 g of NaCl in about 600 ml of
distilled water and dilute to 1 liter.
Stock standard phosphorus solution: Dissolve 0.4393 g of pre-dried
(105°C for 1 hour) KH2P04 in distilled water and dilute to 100 ml.
1.0 mg = .1 mg P.
PROCEDURE
Digestion
a. To 20 or 2.5 ml of sample, add 5 ml of digestion solution and mix
by use of vortex mixer.
b. Add boiling chips (4 to 8 Teflon boiling stones). NOTE: Too
many boiling chips will cause the sample to boil over.
c. Set the low temperature setting at 200°C and the high temperature
setting at 200°C and preheat to 200°C. Place tubes in the digestion
and set the timer for the low temperature for 1 hour and the timer
for the high temperature for 2 1/2 hours. Set the high temperature
setting at 380°C.
***See concentration range, Table 1 of appendices for ml amounts of sodium
hydroxide solution.
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NOTE: If eight inch tubes are used, the high temperature timer
should be set for 30 minutes after the temperature has reached
380°C. Longer time and higher temperature may result in complete
loss of the acid.
d. After the digestion has been completed, cool the samples and add
25 ml of ammonia free water and mix.
Colorimetric Analysis
a. Check the level of all reagent containers to ensure an adequate
supply.
b. Excluding the salicylate and molybdate/antimony lines, place all
reagent lines in their respective containers, connect the sample
probe to the Sampler IV, and start the proportioning pump.
c. Flush the Sample IV wash receptacle with about 25 ml of 4% sulfuric
acid.
d. When the reagents have been pumping for at least 15 minutes, place
the salicylate and molybdate/antimony lines in their respective
containers and allow the system to equilibrate.
NOTE 1: If a precipiate forms after the addition of salicylate,
the pH is too low. Immediately stop the proportioning
pump and flush the coils with water using a syringe.
Before restarting the system, check the concentration of
the sulfuric acid solutions and/or the working buffer
solution.
NOTE 2: To prevent precipitation of sodium salicylate in the
waste tray (which can clog the tray outlet), keep the
nitrogen flowcell pump tube and the nitrogen colorimetric
"To Waste" tube separate from all other lines, or keep
tap water flowing in the waste tray.
e. After a stable baseline has been obtained, start the Sampler.
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SECTION IV
DATA
TECHNICON SYSTEM
To 20 ml of sample 0.01 g of mercuric oxide, 10 ml of cone, sulfuric
acid and 6 g potassium sulfate are added. The samples and standards are
digested for 3 hours. After digestion, the samples are cooled, diluted to
75 ml, and placed on the AutoAnalyzer for ammonia and phosphate determination.
The reliability of this system was determined by analyzing a variety
of organic compounds for nitrogen and phosphorus. Table 2* shows the re-
covery of nitrogen from cysteine and nicotinic acid. The recovery of nitro-
gen from cysteine was equal to the recovery obtained using the total Kjeldahl
nitrogen method (1). The recovery of nitrogen from nicotinic acid using the
total Kjeldahl method was less than 1%; however, with the block digester
system, 52% recovery was obtained from 10 mg per liter. The recovery of
phosphorus and nitrogen from adenosine-5 phosphate was equal to the recovery
obtained using the automated vanadium TKN method (2).
The precision of this method was determined by analyzing 7 replicates
of a sewage sample. The organic nitrogen plus ammonia nitrogen concentration
was 11.4 mg N per liter and the standard deviation was + 0.5. The phosphorus
concentration was 1.1 mg P per liter and the standard deviation was +0.2.
Because of this relatively large standard deviation for phosphorus, 20%, it
was felt that improvement could be made. The fact that 10 ml of cone, sul-
furic are added makes it very difficult to mix the sample after digestion.
The 6 grams of potassium sulfate required for each sample is a considerable
quantity.
MODIFIED METHOD
As an alternate possibility, the digestion solution used for the total
Kjeldahl nitrogen method was tried. With this method only 0.65 g of potas-
sium sulfate and 1 ml of cone, sulfuric acid are required for each sample.
Because only 5 ml of the digestion solution is used, an increase in the
sample size from 20 to 25 ml is possible. Comparison of the Technicon system
and the modified method is shown in Table 4.
In the Technicon method the samples were digested for a total of 3
hours: 1 hour at low temperature, 200°C, and 1 hour at 370°C With this
''For all tables and figures, see the Appendices.
6
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time and temperature about 1.5 hours was required to remove the water from
the samples. With the modified method, the water was evaporated in 1 hour;
therefore, the total elapsed time was reduced to 2.5 hours. It was noted
that all the holes in this block did not have the same temperature. Because
of this variation in temperature, poor precision was obtained for some
compounds. It was also noted that better precision and higher recoveries
of highly refractory compounds, such as nicotinic acid and adenosine-5-
phosphate, were obtained when the high temperature was set at 380°C and the
total time was set at 3 hours (retaining the 1 hour at low temperature).
Jirka and Carter (4) recommended the use of 1 x 8" digestion tubes in
place of 1 x 10" tubes. Table 5 shows the comparison of results obtained
for three concentrations of nicotinic acid with the two types of tubes.
All samples and standards were digested at the same time and analyzed with
the same reagents and colorimeter settings. The digestor was set for 1 hour
at 200°C and total time was 2.5 hours. Higher values were obtained for
samples digested in the* 8-inch tubes. The higher values indicated that the
water was removed from the 8-inch tubes sooner than from the 10-inch tubes.
Therefore, these samples were digested longer. Eight-inch tubes may be used
in place of 10-inch tubes; the digestion must not exceed 30 minutes at 380°C.
Except for the data in Table 5, the other results in this study were obtained
using the 10-inch tubes.
In both the original method and the modified method, the samples were
diluted to 75 ml after digestion. Jirka and Carter-(4) found that greater
sensitivity could be obtained by diluting the samples to 10 ml. This was an
improvement in the method when samples with low concentrations of TKN were
analyzed, but does not provide sufficient sample if a rerun is necessary.
Therefore, for this study the samples were diluted to 25 ml. The 25 ml
sample is sufficient to fill two sample tubes. Table 1 shows the dilution
loops used for various concentration ranges of ammonia. Best results are
obtained when dilution loops 3,4,5 and 6 are used. Figures 1 and 2 show the
manifolds used for the determination of ammonia and phosphate. For this
study, the sampling rate was decreased from 40 per hour (9:1) to 30 per hour
(4:1). The chart speed was 3/16 inch per minute. The salicylate-hypochlor-
ite reaction with ammonia was found to be as sensitive as the phenate-
Basically, only minor changes in Technicon's method for determining
ammonia and phosphate following digestion were made. The sulfuric acid wash
solution was reduced from 13% to 4% and the sulfuric acid in the phosphorus
method was reduced from 2.0 N to 0.72 N because of the smaller amount of
acid used for digestion. The ammoniummolybdate was reduced from 30 g per
liter to 8.0 g per liter because 30 g per liter was found to be an excessive
amount. Two milli.liters of acetone were added to preserve the ascorbic acid
and prevent precipitation in the system.
The reliability of this modified procedure was determined for a solution
of ammonium chloride, a reference sample from EMSL, Quality Assurance Labor-
atory, and several sewage samples. The ammonium chloride was included to
determine if ammonia would be lost during the digestion step. The reference
sample was analyzed to determine the recovery of organic nitrogen. As shown
in Table 6, the coefficients of variation for the two compounds are about
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equal. This reference sample was also added as a spike to sewage samples.
As shown in Table 7, the recovery of phosphate was approximately 93% and the
recovery of organic nitrogen was 92%.
Accuracy was also determined by analyzing several organic compounds for
both nitrogen and phosphorus. Sewage samples were also analyzed for organic
nitrogen plus ammonia and the results compared to those obtained using the
ammonia probe. Table 8 lists the recovery of nitrogen and phosphorus from
two organic compounds (nicotinic acid and adenosine-5-phosphate) added to
distilled water. These samples were digested with the block digester and
analyzed using the colorimetric methods. For nicotinic acid the recovery of
nitrogen was 76% for 0.5 mg N per liter and 71% for 10 mg N per liter. The
average recovery of nitrogen from adenosine-5-phosphate was 85% for the range
of 1.1 to 6.7 mg N per liter. The recovery of phosphorus for the range 0.5
to 3.0 mg per liter was 94%. Table 9 lists the results obtained using the
colorimetric method versus the ammonia probe. The same digested sample was
used for both methods. The probe was used in this set to determine whether
the ammonia mercury complex was broken. Because about the same results
were obtained for the two methods, it was concluded that the complex was
broken.
The precision of this method was determined at three separate concen-
tration levels. The samples used for this study were sewage, two river
waters, and an industrial waste. They included a low and two intermediate
concentrations. The nitrogen concentrations were 5.7, 0.98, and 1.92 mg per
liter. The precision was ±0.11, ±0.03, and ±0.05 mg per liter, respectively.
Jirka and Carter (4) also made a study of the interferences using the
automated phenate and single reagent methods. They found that high concen-
trations of chromium, zinc, copper, vanadium, and manganese can cause low
recovery of nitrogen. High concentrations of chromium will also cause low
recovery of phosphorus. Arsenic is a positive interference for phosphorus.
The same interferences were noted for the salicylate and the two reagent
phosphorus methods. Nitrate also interferes with the TKN when it is present
in concentrations ten times or greater than the TKN levels present(S).
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SECTION V
REFERENCES
1. Methods for Chemical Analysis of Water and Wastes, 1974.
2. Gales, M. E., and Booth, R. L., Simultaneous and Automated Determination
of Total Phosphorus and Total Kjeldahl Nitrogen , Methods Development
and Quality Assurance Research Laboratory, May 1974.
3. Technicon, Total Kjeldahl Nitrogen and Total Phosphorus BD-40 Digestion
Procedure for Water, August 1974.
4. Jirka, A. M., Carter, M. J., May, D., and Fuller, F. D., Ultramiro Semi-
Automated Method for the Simultaneous Determination of Total Phosphorus
and Total Kjeldahl Nitrogen in Wastewaters, to be published. (Can be
obtained from Andrea M. Jirka, Central Regional Laboratory, 1819 W.
Pershing Road, Chicago, Illinois 60609.)
5. Schlueter, A., Nitrate Interference in Total Kjeldahl Nitrogen Deter-
mination and its Removal by Anion Exchange Resins, EPA-600/7-77-017,
Environmental Monitoring and Support Laboratory, Cincinnati, Ohio.
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TABLE 1
CONCENTRATION RANGES
(NITROGEN)
Dilution loops
Initial sample
No.
1
2
3
4
5
6
Sample line
.80 (RED/RED)
.80 (RED/RED)
.16 (ORN/YEL)
.16 (ORN/YEL)
.16 (ORN/YEL)
.16 (ORN/YEL)
Diluent line
.80 (RED/RED)
.80 (RED/RED)
.80 (RED/RED)
.80 (RED/RED)
.80 (RED/ RED)
.80 (RED/ RED)
Resample
Resample line
.32 (BLK/BLK)
.32 (BLK/BLK)
.32 (BLK/BLK)
.32 (BLK/BLK)
.16 (ORN/YEL)
.16 (ORN/YEL)
Diluent line
.80 (RED/RED)
.80 (RED/ RED)
.80 (RED/RED)
.80 (RED/RED)
.80 (RED/RED)
.80 (RED/RED)
Approx .
std.cal.
setting
700
100
700
100
700
100
Range
PPM N
(+10%)
0-0.5
0-1.5
0-1
0-5
0-2
0-10
ml stock NaOH
per liter
working buffer
solution
250
250
120
120
80
80
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TABLE 2
t ,
RECOVERY OF NITROGEN FROM CYSTEINE AND
NICQTINIC ACID WITH THE BLOCK DIGESTOR SYSTEM
Sample
Cysteine
Nicotinic
Sewage
Sewage §
Sewage £
Amounts added
mg N/l
1.0
10.0
1.0
10.0
0
Cysteine 4.0
8.0
Nicotinic 4.0
8.0
mg/1
found
0.96
9.8
0.53
5.20
0.79
4.73
8.74
2.95
4.17
%recovery
96
98
53
52
--
99
99
54
42
TABLE 3
RECOVERY OF PHOSPHORUS AND NITROGEN FROM
ADENOSINE-5-PHOSPHATE WITH THE BLOCK DIGESTOR SYSTEM
Sample
Phosphorus added
mg/1
Phosphorus found
mg/1
Nitrogen added
mg/1
Nitrogen found
mg/1
%recovery
Distilled H20
Sewage
1.0
2.0
5.0
0
2.0
0.9
1.71
3.94
6.90
8.67
90
85
79
--
89
^recovery
Distilled H20
Sewage
0.45
0.90
2.26
4.52
11.30
0
4.5
0.45
0.91
2.10
3.86
9.2
6.90
9.98
100
101
93
85
81
--
68
11
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TABLE 4
COMPARISON OF TECHNICON'S SYSTEM AND THE MODIFIED SYSTEM
Item Technicon Modified
Sample 20 ml 20 or 25
Digestion 10 ml H.,SO, 1 ml H_SO,
24 24
6.3 g K2S04 0.66 g K2S04
.1 g HgO .01 g HgO
Time of digestion 3 hours 2.5 hours
Manifold Technicon Technicon
TABLE 5
COMPARISON OF TKN DATA OBTAINED FOR NICOTINIC
ACID USING THE IX 8" AND IX 10". DIGESTIONTUBES
mg'N/l added 8-inch tubes %recovery 10-inch'tubes %recovery
mg N/l found mg N/l found
1.0
3.0
10.0
0.99
2.70
8.20
9d
90
82
.80
2.48
6.30
80
83
63
TABLE 6
RECOVERY OF AMMONIA FROM AMMONIUM CHLORIDE
AND QAL REFERENCE SAMPLE
Ammonium chloride - Actual value: 2.0 mg N/l
Mean 2.1
Number of samples 32
Standard deviation tO.08
Coefficience of var. 5.9%
Sample from QAL - Actual value: 5.8 mg N/l
Mean 5.6
Number of samples 32
Standard deviation +0.22
Coefficience of var. 4.0%
12
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TABLE ?
RECOVERY OF NITROGEN AND PHOSPHORUS FROM SEWAGE SAMPLES
Total Phosphorus
Sample
1
2
3
Found
mg/1
1.14
1.29
1.17
Added
mg/1
0.71
0.71
0.71
Recovered
mg/1
1.86
1.89
1.84
%recovery
101
85
94
Organic Nitrogen
Sample
1
2
3
Found
mg/1
3.66
1.54
1.33
Added
mg/1
5.25
5.25
5.25
Recovered
mg/1
8.27
6.45
6.30
%recovery
89
93
95
TABLE 8
RECOVERY OF NITROGEN AND PHOSPHORUS FROM
ORGANIC COMPOUNDS ADDED TO OHIO RIVER WATER
Compound added
N in sample
Cone. added
N found
%recovery
Nicotinic acid 0.85
mg/1 0.85
0.85
0.85
Adenosine - 5- phosphateO.85
mg/1 0.85
0.85
0.85
0.5
1.0
5.0
10.0
1.13
2.26
4.50
6.70
1.23
1.53
4.27
7.90
1.80
2.66
4.77
6.79
76
68
68
71
84
80
87
89
P in sample
Cone. added
P found %recovery
AJ r . 0-06
Adenosine - 5 -phosphate Q Q6
mg/1 0:06
0.06
0.5
1.0
2.0
3.0
0.55
1.00
1.94
2.78
98
94
94
91
13
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TABLE 9
COMPARISON OF NITROGEN RESULTS,
COLORIMETRIC METHOD VS. THE AMMONIA PROBE, MG N/l
Sample Colorimetric Method Ammonia Probe
1 10 11.2
2 1.2 1.3
3 2.6 2.2
4 1.7 1.6
14
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ml/min
GRY GRY 1.0 4% H2SO4
10 TURNS
OQQO
116-0489-01
37 °C
5 TURNS 157-B273-03 10 TURNS
0000 I Oooo I 0000
"G" COIL
157-B089
20 TURNS
OOOQ
TO PUMP TUBE
BLK BLK
RED RED
ORN YEL
BLK BLK
RED RED
ORN YEL
BLK BLK
ORN YEL
GRY GRY
0.32 AIR
0.80 DILUENT WATER
TO PHOSPHORUS
SAMPLE LINE
•SAMPLE
116-BOOO
0.32 AIR
0.80 WORKING BUFFER
•RESAMPLE
0.32 SALICYLATE-NITROPRUSSIDE
0.16 HYPOCHLORITE
WASTE
1.0 WASTE
•SEE CHART FOR RANGE SELECTION (Table 1
COLORIMETER
660nm
50mm F/C * 1.5mm ID
FIGURE 1. AMMONIA MANIFOLD AAil
-------
10 TURNS
116-0489-01
5 TURNS
0000
37°C
157-13273-03
0000
10 TURNS
0000
20 TURNS
157-B089
0000
WASTE
TO PUMP TUBE
COLORIMETER
660 nm
50mm F/C x 1.5mm ID
BLK BLK
WHT WHT
ORN ORN
BLK BLK
WHT WHT
ORN YEL
BLK BLK
BLK BLK
YEL YEL
ml/min
0.32 AIR
0.60 NaCI SOLUTION
0.42 SAMPLE
0.32 AIR
0.60 ACID SOLUTION
0.16 RESAMPLE
0.32 MOLYBDATE-ANTIMONY
0.32 ASCORBIC ACID
1.2 WASTE
FIGURE 2. PHOSPHORUS MANIFOLD AA11
TO WASTE
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TECHNICAL REPORT DATA
(Please read Instructions on the reverse before completing)
1. REPORT NO.
EPA-600/4-78-015
2.
3. RECIPIENT'S ACCESSION-NO.
4. TITLE AND SUBTITLE
EVALUATION OF THE TECHNICON BLOCK DIGESTOR SYSTEM
FOR TOTAL KJELDAHL NITROGEN AND TOTAL PHOSPHORUS
5. REPORT DATE
February 1978 issuing date
6. PERFORMING ORGANIZATION CODE
7. AUTHOR(S)
Morris E. Gales, Jr. and Robert L. Booth
8. PERFORMING ORGANIZATION REPORT NO.
9. PERFORMING ORGANIZATION NAME AND ADDRESS
Environmental Monitoring and Support Laboratory- OH'
Office of Research and Development
U.S. Environmental Protection Agency
Cincinnati, Ohio 45268
10. PROGRAM ELEMENT NO.
1BD612
11. CONTRACT/GRANT NO.
12. SPONSORING AGENCY NAME AND ADDRESS
Same as above
13. TYPE OF REPORT AND PERIOD COVERED
In-House
14. SPONSORING AGENCY CODE
EPA/600/06
15. SUPPLEMENTARY NOTES
16. ABSTRACT
Technicon's block digestor method for the simultaneous determination of total
phosphorus and total Kjeldahl nitrogen has been evaluated and modified for the
semi-automated determination of these constituents in surface water and domestic
and industrial wastes. The Technicon digestion mixture was replaced with the
Kjeldahl nitrogen digestion solution. The applicable range is 0.1 to 20 mg per
liter for phosphorus and nitrogen.
17.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
b.lDENTIFIERS/OPEN ENDED TERMS
c. cos AT I Field/Group
Automation
Nutrients
Nitrogen
Phosphorus compounds
Nitrogen compounds
Analytical techniques
Color reactions
Phosphorus chemical
analysis
99 A
18. DISTRIBUTION STATEMENT
RELEASE TO PUBLIC
19. SECURITY CLASS (ThisReport)
UNCLASSIFIED
21. NO. OF PAGES
23
20. SECURITY CLASS (This page)
IIMn.ASSTFTFn
22. PRICE
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T7
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