Professional Documents
Culture Documents
D888 137950 1 PDF
D888 137950 1 PDF
1. Scope
1.1 These test methods cover the determination of dissolved
oxygen in water. Three test methods are given as follows:
Test Method ATitrimetric Procedure
High Level
Test Method BInstrumental Probe Procedure
Electrochemical
Test Method CInstrumental Probe Procedure
Luminescence-Based Sensor
Range, mg/L
>1.0
Sections
8 to 15
0.05 to 20
16 to 25
0.05 to 20
26 to 29
1
These test methods are under the jurisdiction of ASTM Committee D19 on
Water and are the direct responsibility of Subcommittee D19.05 on Inorganic
Constituents in Water.
Current edition approved March 1, 2012. Published March 2012. Originally
approved in 1946. Last previous edition approved in 2009 as D888 09. DOI:
10.1520/D0888-12.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standards Document Summary page on
the ASTM website.
3
Reagent Chemicals, American Chemical Society Specifications , American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD.
Copyright. (C) ASTM International, 100 Barr Harbour Drive P.O. box C700 West Conshohocken, Pennsylvania 19428-2959, United States
Copyright by ASTM Int'l (all rights reserved); Mon Jul 23 06:27:53 EDT 2012
1
Downloaded/printed by
(Book Supply Bureau) pursuant to License Agreement. No further reproductions authorized.
SUPPLIED BY BSB UNDER LICENCE FROM ASTM FOR KALYANI ALSTOM POWER LIMITED - NOIDA ON 24/07/2012
This standard is issued under the fixed designation D888; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon () indicates an editorial change since the last revision or reapproval.
D888 12
6. Sampling
6.1 Collect the samples in accordance with Practices D1066
and D3370.
6.2 For higher concentration of dissolved oxygen, collect
the samples in narrow mouth glass-stoppered bottles of
300-mL capacity, taking care to prevent entrainment or solution of atmospheric oxygen.
6.3 With water under pressure, connect a tube of inert
material to the inlet and extend the tube outlet to the bottom of
the sample bottle. Use stainless steel, Type 304 or 316, or glass
tubing with short neoprene connections. Do not use copper
tubing, long sections of neoprene tubing, or other types of
polymeric materials. The sample line shall contain a suitable
cooling coil if the water being sampled is above room
temperature, in which case cool the sample 16 to 18C. When
a cooling coil is used, the valve for cooling water adjustment
shall be at the inlet to the cooling coil, and the overflow shall
be to a point of lower elevation. The valve for adjusting the
flow of sample shall be at the outlet from the cooling coil. The
sample flow shall be adjusted to a rate that will fill the sampling
vessel or vessels in 40 to 60 s and flow long enough to provide
a minimum of ten changes of water in the sample vessel. If the
sampling line is used intermittently, flush the sample line and
cooling coil adequately before using.
6.4 Where samples are collected at varying depths from the
surface, a special sample bottle holder or weighted sampler
with a removable air tight cover should be used. This unit may
be designed to collect several 250 or 300 mL samples at the
same time. Inlet tubes extending to the bottom of each bottle
and the water after passing through the sample bottle or bottles
displaces air from the container. When bubbles stop rising from
the sampler, the unit is filled. Water temperature is measured in
the excess water in the sampler.
6.5 For depths greater than 2 m, use a Kemmerer-type
sampler. Bleed the sample from the bottom of the sampler
through a tube extending to the bottom of a 250 to 300 mL
biological oxygen demand (BOD) bottle. Fill the bottle to
overflowing and prevent turbulence and the formation of
bubbles while filling the bottle.
7. Preservation of Samples
7.1 Do not delay the determination of dissolved oxygen.
Samples for Test Method A may be preserved 4 to 8 h by
adding 0.7 mL of concentrated sulfuric acid (sp gr 1.84) and
1.0 mL of sodium azide solution (20 g/L) to the bottle
containing the sample in which dissolved oxygen is to be
determined. Biological activity will be inhibited and the
dissolved oxygen retained by storing at the temperature of
Copyright by ASTM Int'l (all rights reserved); Mon Jul 23 06:27:53 EDT 2012
2
Downloaded/printed by
(Book Supply Bureau) pursuant to License Agreement. No further reproductions authorized.
SUPPLIED BY BSB UNDER LICENCE FROM ASTM FOR KALYANI ALSTOM POWER LIMITED - NOIDA ON 24/07/2012
D888 12
Copyright by ASTM Int'l (all rights reserved); Mon Jul 23 06:27:53 EDT 2012
3
Downloaded/printed by
(Book Supply Bureau) pursuant to License Agreement. No further reproductions authorized.
SUPPLIED BY BSB UNDER LICENCE FROM ASTM FOR KALYANI ALSTOM POWER LIMITED - NOIDA ON 24/07/2012
4
Carpenter, J. H., New Measurement of Oxygen Solubility in Pure and Natural
Water, Limnology and Oceanography, Vol 11, No. 2, April 1966, pp. 264277.
5
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report D191070.
13. Calculation
13.1 Calculate the dissolved oxygen content of the sample
as follows:
Dissolved oxygen, mg/L 5
T 3 0.2
200 3 1000
(1)
where:
T = 0.025 N titrating solution required for titration of the
sample, mL.
13.2 Use Eq 2 to convert to a standard temperature and
pressure measurement.
A
Dissolved oxygen, mg/L 5 0.698
(2)
where:
A = oxygen at 0C and 760 mm Hg, mL.
Copyright by ASTM Int'l (all rights reserved); Mon Jul 23 06:27:53 EDT 2012
4
Downloaded/printed by
(Book Supply Bureau) pursuant to License Agreement. No further reproductions authorized.
SUPPLIED BY BSB UNDER LICENCE FROM ASTM FOR KALYANI ALSTOM POWER LIMITED - NOIDA ON 24/07/2012
D888 12
D888 12
TEST METHOD B
INSTRUMENTAL PROBE PROCEDURE
ELECTROCHEMICAL
16. Scope
16.1 This test method is applicable to waters containing
dissolved oxygen in the range from 50 to 20 000 g/L. It is the
users responsibility to ensure the validity of this test method
for waters of untested matrices.
16.2 This test method describes procedures that utilize
electrochemical probes for the determination of dissolved
oxygen in fresh water and in brackish and marine waters that
may contain dissolved or suspended solids. Samples can be
analyzed in situ in bodies of water or in streams, or samples
can be collected and analyzed subsequent to collection. The
electrochemical probe method is especially useful in the
monitoring of water systems in which it is desired to obtain a
continuous record of the dissolved oxygen content.
16.2.1 This test method is recommended for measuring
dissolved oxygen in waters containing materials that interfere
with the chemical methods, such as sulfite, thiosulfate, polythionate, mercaptans, oxidizing metal ions, hypochlorite, and
organic substances readily hydrolyzable in alkaline solutions.
16.3 Electrochemical dissolved oxygen probes are practical
for the continuous monitoring of dissolved oxygen content in
natural waters, process streams, biological processes, etc.,
when the probe output is conditioned by a suitably stable
electronic circuit and recorded. The probe must be standardized before use on samples free of interfering materials,
preferably with the azide modification of Test Method A.
17. Summary of Test Method
17.1 The most common instrumental probes for determination of oxygen dissolved in water are dependent upon electro-
Copyright by ASTM Int'l (all rights reserved); Mon Jul 23 06:27:53 EDT 2012
5
Downloaded/printed by
(Book Supply Bureau) pursuant to License Agreement. No further reproductions authorized.
SUPPLIED BY BSB UNDER LICENCE FROM ASTM FOR KALYANI ALSTOM POWER LIMITED - NOIDA ON 24/07/2012
Copyright by ASTM Int'l (all rights reserved); Mon Jul 23 06:27:53 EDT 2012
6
Downloaded/printed by
(Book Supply Bureau) pursuant to License Agreement. No further reproductions authorized.
SUPPLIED BY BSB UNDER LICENCE FROM ASTM FOR KALYANI ALSTOM POWER LIMITED - NOIDA ON 24/07/2012
D888 12
D888 12
Log y 5 B / T 1 A
(3)
where:
y = scale factor, milligrams of dissolved oxygen per litre
per microampere of electrode current,
B = slope constant,
T = temperature, C, and
A = intercept constant.
This relationship is linear on a semilog plot only over a range
of 610C. Over larger ranges an equation of higher degree is
necessary to reflect the curvature of the relationship.
20.3.2 If the thallium probe is utilized in a circuit without
temperature compensation, the observed output in millivolts
must be corrected for the temperature sensitivity of the
measuring cell that has a temperature coefficient of 1.0 mV/C.
The measuring cells output will increase (apparent dissolved
oxygen concentration decrease) with an increase in temperature,
MVR 5 MV0 2 1.0 ~To 2 TR!
(4)
where:
MVR = millivolts of output at reference temperature,
MV0 = millivolts of output observed,
= reference temperature, C, and
TR
= temperature at the observed output, C.
To
20.4 Correction for Content of Dissolved SaltsIf the
concentration of salts is above 1000 mg/L, it will be necessary
to correct for the effect of the salts in the relationship between
oxygen partial pressure and concentration and also for the
activity of thallium ion. For any given salt, a series of
experimental data should be obtained in which solutions are
prepared by dissolving varying weights of the salt in reagent
water in the range of interest. The solutions plus a reagent
water control are aerated at constant temperature until oxygen
saturation is achieved. Determine the oxygen concentration of
each solution by the chemical method and, at the same time,
obtain probe readings. Determine the ratio A for each solution
as follows:
A5O/R
(5)
where:
O = actual dissolved oxygen concentration, mg/L, as determined by Test Method A, and
R = reading of the probe meter.
For the reagent water control to which the probe is calibrated, the value of A is 1.0. Prepare a plot with salt
concentration as abscissa and the ratio A as ordinate. Use the
developed curve for calculation of the dissolved oxygen
content of salt waters.
21. Sampling
21.1 Bottle SamplesCollect a bottle sample by the procedure described in Practice D1066 or Practices D3370. Collect
the samples in 300-mL BOD bottles or other suitable glassstoppered bottles, preventing entrainment or solution of atmospheric oxygen. If analysis is delayed beyond 15 min, cool the
sample below 5C and hold at this temperature until analyzed.
Make the dissolved oxygen determination without further
temperature adjustment using the appropriate temperature
coefficient. It will be necessary to have the probe at the
temperature of the sample or otherwise compensate for instability due to heat flow from probe to sample.
21.2 In Situ SamplesAn effective use of the instrumental
probes is for the direct, in situ determination of dissolved
oxygen. By this means, sample handling problems are avoided,
and data may be obtained quickly at various locations in a body
of water without concern for the change in oxygen during
storage or handling.
22. Procedure
22.1 Consider carefully the manufacturers recommendations on the use of equipment to obtain satisfactory operation.
22.2 Provide for suitable turbulent flow past the membrane
of membrane probes or past the thallium probe. This may,
under some circumstances, be achieved adequately in flowing
streams. However, in large bodies of water, it may be necessary
to employ mechanical stirring or pumping of water past the
probe. For accurate results, it is important that comparable
degrees of turbulence be employed both for calibration and
utilization.
22.3 If the probe is not automatically compensated for
temperature changes, record the temperature of the water at the
sample probe at the time of dissolved oxygen measurement. To
avoid heat-flow effects, it is important that temperature equilibrium be established between sample and probe.
22.4 Recalibrate the probe whenever the comparison with
reference samples (20.2) indicates an absolute error of more
than 60.2 mg/L of dissolved oxygen or other value that is
compatible with the desired accuracy.
22.4.1 Careful handling is required with membrane probes
to avoid rupturing the thin membrane.
22.4.2 Recalibrate the probe after replacing the membrane
or cleaning the probe in accordance with the manufacturers
directions. For a period of a few hours after a membrane
replacement, the probe output may drift, and frequent recalibration may be required.
Copyright by ASTM Int'l (all rights reserved); Mon Jul 23 06:27:53 EDT 2012
7
Downloaded/printed by
(Book Supply Bureau) pursuant to License Agreement. No further reproductions authorized.
SUPPLIED BY BSB UNDER LICENCE FROM ASTM FOR KALYANI ALSTOM POWER LIMITED - NOIDA ON 24/07/2012
Copyright by ASTM Int'l (all rights reserved); Mon Jul 23 06:27:53 EDT 2012
8
Downloaded/printed by
(Book Supply Bureau) pursuant to License Agreement. No further reproductions authorized.
SUPPLIED BY BSB UNDER LICENCE FROM ASTM FOR KALYANI ALSTOM POWER LIMITED - NOIDA ON 24/07/2012
D888 12
SUPPLIED BY BSB UNDER LICENCE FROM ASTM FOR KALYANI ALSTOM POWER LIMITED - NOIDA ON 24/07/2012
D888 12
D888 12
DO Conc.
(mg/L)
Low
High
1.72 1.74
7.22 9.23
104.0
104.0
1.75
1.10
Data Set 1
Data Set 2
Method A
Method B Method C Method A Method B Method C
Winkler % Rec.Membrane LDO % Rec. Winkler Membrane LDO % Rec.
% Rec.
% Rec.
% Rec.
1
88.2
95.7
96..7
96.1
99.4
96.0
97.5
98.9
98.2
97.5
98.9
98.9
97.9
99.0
101.0
98.7
98.9
99.2
99.9
98.1
99.2
97.4
97.7
99.5
96.7
96.6
100.0
91.0
90.6
101.0
94.3
94.3
101.0
94.5
94.5
98.4
95.0
96.1
101.0
96.2
96.2
99.6
104.0
109.0
104.0
107.0
106.0
105.0
10
93.2
90.8
98.6
93.8
94.8
94.8
11
104.0
104.0
102.0
105.0
97.9
102.0
Average
97.5
97.7
101.0
97.6
97.4
99.3
Stdev
5.6
4.0
2.9
4.7
3.8
2.7
%RSD
5.8
4.1
2.9
4.8
3.9
2.7
97.6
97.5
100.0
Stdev
5.0
3.8
2.7
%RSD
5.2
3.9
2.7
Copyright by ASTM Int'l (all rights reserved); Mon Jul 23 06:27:53 EDT 2012
10
Downloaded/printed by
(Book Supply Bureau) pursuant to License Agreement. No further reproductions authorized.
SUPPLIED BY BSB UNDER LICENCE FROM ASTM FOR KALYANI ALSTOM POWER LIMITED - NOIDA ON 24/07/2012
D888 12
31.7.1 Independent reference water samples may be obtained from commercial sources. The value obtained from
these samples must fall within the control limits established by
the commercial source.
31.8 Table 1 and Table 2 reflect round robin results that a
typical user of this method should achieve.
32. Keywords
32.1 analysis; dissolved oxygen; frequency domain;
lifetime-based; luminescence; probe; titrimetric; water
(Nonmandatory Information)
X1. OXYGEN SATURATION VALUES
Temperature,
C
1000
2000
3000
4000
5000
0
2
4
6
8
10
12
14
16
18
20
22
24
26
28
30
32
34
36
38
40
14.6
13.8
13.1
12.4
11.8
11.3
10.8
10.3
9.9
9.5
9.1
8.7
8.4
8.1
7.8
7.5
7.3
7.1
6.8
6.6
6.4
14.1
13.3
12.7
12.0
11.4
10.9
10.4
9.9
9.7
9.2
8.8
8.4
8.1
7.8
7.5
7.2
7.1
6.9
6.6
6.4
6.2
13.6
12.9
12.2
11.6
11.0
10.5
10.1
9.6
9.2
8.7
8.5
8.1
7.8
7.6
7.3
7.0
6.8
6.6
6.3
6.2
6.0
13.2
12.4
11.9
11.2
10.6
10.2
9.7
9.3
8.9
8.6
8.2
7.8
7.6
7.3
7.0
6.8
6.6
6.4
6.1
5.9
5.8
12.7
12.0
11.4
10.8
10.3
9.8
9.4
9.0
8.6
8.3
7.9
7.7
7.3
7.0
6.8
6.5
6.4
6.2
5.9
5.7
5.6
12.3
11.6
11.0
10.4
9.9
9.5
9.1
8.7
8.3
8.0
7.7
7.3
7.1
6.8
6.6
6.3
6.1
6.0
5.7
5.6
5.4
Chlorinity, %
6000
Temperature,
C
4.0
8.0
12.0
16.0
20.0
11.8
11.2
10.6
10.1
9.6
9.2
8.8
8.3
8.0
7.7
7.4
7.1
6.8
6.6
6.3
6.1
5.9
5.8
5.5
5.4
5.2
0
2
4
6
8
10
12
14
16
18
20
22
24
26
28
30
32
34
36
38
40
14.6
13.8
13.1
12.4
11.8
11.3
10.8
10.3
9.9
9.5
9.1
8.7
8.4
8.1
7.8
7.5
7.3
7.1
6.8
6.6
6.4
13.9
13.2
12.5
11.8
11.3
10.8
10.3
9.9
9.4
9.1
8.7
8.4
8.1
7.8
7.5
7.2
7.0
6.8
6.6
6.4
6.2
13.2
12.5
11.9
11.3
10.8
10.3
9.8
9.4
9.0
8.7
8.3
8.0
7.7
7.5
7.2
7.0
6.7
6.5
6.3
6.1
5.9
12.5
11.9
11.3
10.8
10.3
9.8
9.4
9.0
8.6
8.3
8.0
7.7
7.4
7.2
6.9
6.7
6.5
6.3
6.1
5.9
5.7
11.9
11.4
10.8
10.3
9.8
9.4
9.0
8.6
8.3
8.0
7.7
7.4
7.1
6.9
6.6
6.4
6.2
6.0
5.8
5.6
5.4
11.3
10.8
10.3
9.8
9.4
9.0
8.6
8.3
8.0
7.6
7.4
7.1
6.9
6.6
6.4
6.2
6.0
5.8
5.6
5.4
5.2
Copyright by ASTM Int'l (all rights reserved); Mon Jul 23 06:27:53 EDT 2012
11
Downloaded/printed by
(Book Supply Bureau) pursuant to License Agreement. No further reproductions authorized.
SUPPLIED BY BSB UNDER LICENCE FROM ASTM FOR KALYANI ALSTOM POWER LIMITED - NOIDA ON 24/07/2012
APPENDIXES
D888 12
TABLE X2.1 Single Operator Recovery and Precision Criteria for Luminescence-based Sensor Two-point Calibration
Single Point Calibration in Air Saturated Water (Saturated solution
placed in BOD bottles and capped)
Two Point Calibration in Air Saturated Water (BOD) and Nitrogen
Saturated Water
Two Point Calibration in Air Saturated Water (BOD) and Sodium
Sulfite
Single Point Calibration in Air Saturated Water (Saturated solution in
a bubbler)
Two Point Calibration in Air Saturated Water (Bubbler) and Nitrogen
Saturated Water
Two Point Calibration in Air Saturated Water (Bubbler) and Sodium
Sulfite
Single Point Calibration in Water Saturated Air
Two Point Calibration in Water Saturated Air and Nitrogen Saturated
Water
Two Point Calibration in Water Saturated Air and Sodium Sulfite
ASW (BOD) / N2
ASW (BOD) / Na2SO3
ASW (Bubbler)
ASW (Bubbler) / N2
ASW (Bubbler) / Na2SO3
WSA
WSA / N2
WSA / Na2SO3
Calibration Method
Test point
Average RDO reading
Stdev
% RSD
Calibration Method
Test point
Average RDO reading
Stdev
% RSD
Calibration Method
Test point
Average RDO reading
Stdev
% RSD
ASW (BOD)
100.0%
99.46%
1.05%
1.05%
Temp
26.83
ASW (Bubbler)
100.0%
99.21%
1.02%
1.03%
Temp
26.83
Temp
26.83
WSA
100.0%
99.18%
1.04%
1.05%
ASW (BOD) / N2
100.0%
99.34%
1.02%
1.03%
ASW (Bubbler) / N2
100.0%
99.17%
1.03%
1.04%
WSA / N2
100.0%
99.20%
1.04%
1.05%
ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.
This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/
COPYRIGHT/).
Copyright by ASTM Int'l (all rights reserved); Mon Jul 23 06:27:53 EDT 2012
12
Downloaded/printed by
(Book Supply Bureau) pursuant to License Agreement. No further reproductions authorized.
SUPPLIED BY BSB UNDER LICENCE FROM ASTM FOR KALYANI ALSTOM POWER LIMITED - NOIDA ON 24/07/2012
Key
ASW (BOD)