UNCON TROLLED

VEST VALLEY NUCLEAR 'SERVICES CO., INC. - 1

- - . / ~~~ACM-DEN1-180L,-Jev.1
ANAIXTICAL CISTRY 'SHOD EffEectiveDate: 06/28/89
ANAKTCAL MAD PROCESS CHEMI STRY,

/ETE1MINAIION OF DENSITY EITH TH

PAAR DIGITAL DENSITY METER.

Approved by:

(6n ,J Vt LUc
C. V. McVay, Manager
Analytical and Process

Part I

1.0 PURPOSE .

> 1.1 To establish a method for the determination of density on various

aqueous samples. -

2.0 APPLICATION

> 2.1 This method is designed for the determination of the density of
aqueous and organic liquids. Exceptions are liquids that attack
the glass oscillator. Hydrofluoric acid is particularly
destructive. The volume -of the oscillator is 0.6 mL; therefore,
the.minimum sample volume is l.mL. In routine~use, the precision
of this method is~approximately i-0.001 density units.

3.0 DISCUSSION

> 3.1 'The Paar'density.meter determines density by-measuring the

deviation in resonant frequency,ofa:hollow glass mechanical
oscillator when filled with sample'material. The volume of the
oscillator is'constant and anychange in its,frequency is due to
.the sample. -

> 3.2 Deleted

3.3 The major sources of error in the analysis are (a) air bubbles in
the oscillator; (b) incompletely filled oscillator; and (c) air
flowing through:the oscillator when obtaining the air reading for
..calibration. -

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~DR~
PROJ PDC I
 AQK-DEN-1801, Rev. I
Effectdve Date: 06/28/89

4.0 REFERENCES

4.1. Calculating Density Meter Instruction Manual, Anton Paar

Part II

5.0 EQUIPMENT

> 5.1 Par Model DHAl-46 Digital Density Meter

> 5.2 Calibrated thermometer

> 5.3 Eyedroppers/syringes

6.0 REAGENTS AND STANDARDS

6.1 Isopropyl Alcohol

6.2 Distilled water

> 6.3 Simulated Supernatant

6.4 0.5 percent hydrofluoric acid. (To be used only as cleaning agent
for very short periods of time.)

7.0 SAFETY PRECAUTIONS

Follow standard safety procedures and specifically do not analyze

uncomplexed hydrofluoric acid solutions per ACP 7.2.

8.0 RECORDS

> 8.1 All measurement data and sample identification shall be recorded
on the work sheet (Attachment B). The final result shall be
recorded on the analytical request sheet per PRD 5.0.

9.0 CALIBRATION AND CONTROL

9.1 See Calculating Density Meter Instruction Manual, Anton Paar,

Pages 6 and 7, Attachment A.

> 9.2 Calibration of the density meter is done by using air and ultra-
pure water. As both air and water have specific density values,
quality control is assured by calibrating the density meter by
using the known values of each. Constants A and B are recorded on
QC charts each time instrument is calibrated.

> 9.3 Air and.water densities-shall be checked and recorded on each day
the instrument is used. When density values are out of limits for
air and ultrapure water, calibration is necessary and the
constants are recorded.

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 ACK-DEN-1801, Rev. 1
Effective Date: 06/28/89

> 9.4 A quality control sample which has a density within 0.5 g/cc of
the density of samples to be analyzed shall be checked and
recorded on each day the instrument is used or at a rate of one in
twenty samples in each set whichever is more frequent.
Recalibration is required if the QC sample is out of tolerance.

10.0 PROCEDURE

10.1 Calibration

> 10.1.1 Calibrate the instrument using air and water as

calibration standards. See Attachment A.

> 10.1.2 Deleted

10.2 Measurements

> 10.2.1 Read the temperature of the oscillator unit. The

temperature should be 20.0 * 0.3 0 C.

> 10.2.2 Calibrate the density meter as in Attachment A, if needed,

see 9.3.

> 10.2.3 Clean the oscillator with water. Additional cleaning

agents are isopropyl alcohol, simulated supernatant, and
5 percent hydrofluoric acid solution.

CAUTION: When using.5 percent HF leave in oscillator for

a maximum of 1 minute.

Air dry until a reading taken on the density meter agrees

with the air reading taken for calibration. This assures
that the oscillator is dry.

> 10.2.4 With a syringe or eye dropper, slowly inject the sample
into the glass oscillator until it is completely filled.
Use light to be certain no air bubbles are present and
oscillator is completely filled. Turn light off so
instrument is able to reach constant temperature of
20.0 *0.30C.

> 10.2.5 Take two readings at 30 second intervals. The readings

will agree within *1 in the last place when constant
temperature is reached. Clean oscillator as per step
10.2.3 and repeat sample analysis.

> 10.2.6 Record the sample readings and calculate average

density. Report four significant figures e.g., 1.415.

10.2.7 Clean the oscillator as per step 10.2.3.

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11.0 CALCULATIONS

> 11.1 Record the data, report four significant figures.

12.0 ATTACHMENTS

Attachment A - Calibration of the Density Meter

> Attachment B - Density Work sheet

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 ACH-DEN-1801, Rev. 1
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ATTACHMENT A

CALIBRATION OF THE DENSITY METER

The apparatus constants, A and B have to be determined and entered into the
constant memories. Both constants are temperature dependent. They have to be
redetermined when the measuring temperature is changed. At no change of the
measuring temperature it is enough to check the calibration value in time
intervals of several weeks.

For the calculation of the constant values, the 4-position switch (display
.selector) is set to IT'; then the period of oscillation IT" is shown on the
display. Now, approximately 0.7 mL distilled water is injected through the
lower opening of the oscillator cell using a plastic tipped hypodermic
syringe. The proper filling of the sample tube may be observed through the
window after the light is switched on., The cell is correctly filled, when the
liquid has passed into the upper (larger) diameter of the sample tube.
Overfilling will have no effect on the proper result.

The syringe may be left in the filling position. The upper opening may be
closed with a teflon plug, for highly volatile substances. The sample must be
; homogeneous and free of even the smallest bubbles.

The light is now switched off, and temperature equilibrium is reached when the
number at the display remains the same within one digit at the fourth place.
This TH 0 value is the period of oscillation of a water-filled oscillator.
At this very first measurement, the sample should remain in the oscillator
cell for about 15 minutes and the T-value should be observed. Now remove the
teflon plug and withdraw the sample into the syringe. rinse the sample tube
with alcohol, acetone, or a similar solvent. Then with the air pump switched
on, connect the air hose to the upper inlet of the sample tube and continue
the flow of air until the displayed value repeats itself several times.
Switch off the pump and compare Tair with its original value. If it is not
identical with the original reading, the oscillator should be rinsed out again
and thoroughly dried to ensure complete removal of all solvent or any other
contamination.

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AQI-DEK-1801, Rev. 1
Effective Data: 06/28/89

I J-~

Now with the density values for air and water, and the corresponding T-values,
the apparatus constants A and B are calculated as follows:
I.
2 2

air air

These values and their corresponding measuring temperature are marked down on
^ the 'inside of the lid (in penc-il)' which covers the constants storage switches.

The constants A and B'are entered into the memory by setting the corresponding
numerical switches on top of the instrument and checked by setting the display
selector switch accordingly. After setting the display selector switch to "p"
the instrument is ready'to work and the density p of a sample is shown on the
display and may be read out from the digital data output.

1,

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I~.I
 AQ-DEN-1801, Rev. 1

ACK-DEN-1801, Rev. 1
Effective. Date: 06/28/89

ATTACHMENT B Page _ of _

DENSITY WORK SHEET

SAMPLE NAME LOG NUMBER

SPECIAL INSTRUCTIONS

I
SAMPLE ID I
,I
I
WATER DENSITY I I
I I
AIR DENSITY I I
I
I
I
I
I
I
AVERAGE SAMPLE I I
DENSITY I I
(g/cc at 200C) I I

CALIBRATED INSTRUMENT USED:

ANALYST DATE

APPROVED DATE

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