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Method 8140

DEHA (0 to 500 µg/L ) For boiler feedwater/condensate


Iron Reduction Method for Oxygen Scavengers*

1. Enter the stored 2. Press: 25 ENTER 3. Fill a sample cell 4. Fill a second sample
program number for The display will show with 25 mL of sample cell with 25 mL of
diethylhydroxylamine µg/L, DEHA and the (the prepared sample). deionized water
(DEHA). ZERO icon. Note: The sample (the blank).
temperature should be
Press: PRGM Note: To prevent
contamination from iron 25 ±3°C (77 ±5 °F).
The display will show:
deposits, rinse sampling Note: When testing for
PRGM ? containers and sample cells compounds that react
Note: To determine other with 1:1 Hydrochloric Acid quickly with oxygen at
oxygen scavengers, Solution. Follow with room temperature, stopper
multiply the result by the several rinsings of the cell containing the
appropriate factor. See deionized water. sample in Steps 5–11.
Other Oxygen Scavengers Note: Samples must be
following these steps. analyzed immediately.

* Adapted from Ishii and Koh, Buneseki Kagaku, 28 473 (1979)

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DEHA (N,N-DIETHYLHYDROXYLAMINE), continued

5. Add the contents of 6. Add exactly 0.5 mL 7. Immediately, press: 8. Immediately after
one DEHA Reagent 1 of DEHA Reagent 2 TIMER ENTER the timer beeps, place
Powder Pillow to each Solution to each sample the blank into the cell
A 10-minute reaction
sample cell. Cap. Swirl cell. Cap and swirl to holder. Tightly cover the
period will begin. For
to mix. mix. Place both sample sample cell with the
hydroquinone, allow
cells in the dark. instrument cap.
only a two-minute
Note: A purple color will reaction period.
slowly develop if DEHA
is present. Note: Both sample cells
must remain in the dark for
the entire reaction period.
Note: Temperature and
reaction time affect results.

9. Press: ZERO 10. Immediately place 11. Press: READ Ferrous Iron Adjustment
The cursor will move to the prepared sample into The cursor will move to Note: Repeat the above
the right, then the the cell holder. Tightly the right, then the result procedure, but do not add
display will show: cover the sample cell in µg/L DEHA will be DEHA Reagent 2 (Step 6)
with the instrument cap. to determine the ferrous
0 µg/L DEHA displayed.
iron content in the sample.
Note: If the display flashes Then press SETUP, scroll
“limit” it is due to high to “BLANK” and press
DEHA levels. Dilute a fresh ENTER. The display will
sample with deoxygenated show; “BLANK?” Enter
deionized water and repeat the blank value just read.
the test. Multiply the result Press ENTER to accept the
by the dilution factor; see value as the blank to be
Section 1. subtracted from
each reading.

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DEHA (N,N-DIETHYLHYDROXYLAMINE), continued
Sampling and Storage
Most oxygen scavengers will react quickly with atmospheric
oxygen. Collect samples in acid-rinsed plastic or glass containers,
allowing the sample to overflow. Cap the container so there is no
head space above the sample. Rinse each sample cell several
times with sample, then carefully fill to the fill mark. Analyze the
sample immediately.
Other Oxygen Scavengers
To determine other oxygen scavengers, perform the test as
directed above, then multiply the DEHA result by the appropriate
factor below:

Oxygen Scavenger Factor


Erythorbic Acid 3.5
(Iso-ascorbic acid)
Hydroquinone 2.5
Methylethylketoxime (MEKO) 4.1
Carbohydrazide 1.3

Method Performance
Precision
In a single laboratory, using a standard solution of 242 µg/L
DEHA and two representative lots of reagent with the instrument,
a single operator obtained a standard deviation of ±6.2 µg/L
DEHA.
Estimated Detection Limit
The estimated detection limit for program 25 is 9 µg/L DEHA.
For more information on the estimated detection limit, see
Section 1.
Interferences
Substances which reduce ferric iron will interfere. Substances
which complex iron strongly may also interfere. Light interferes
with the color development. The following may also interfere
when present in concentrations exceeding those listed below:
Borate (as Na2B4O7) 500 mg/L Molybdenum 80 mg/L
Cobalt 0.025 mg/L Nickel 0.8 mg/L
Copper 8.0 mg/L Phosphate 10 mg/L
Hardness (as CaCO3) 1000 mg/L Phosphonates 10 mg/L
Lignosulfonates 0.05 mg/L Sulfate 1000 mg/L
Manganese 0.8 mg/L Zinc 50 mg/L

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