U. 8.

DEPARTMENT OF THE INTERIOR

Geololical Survey
Water Ruourcea .Diviaion

WubiDrton, D. C.

fLAME PHOTOMETRIC DETERMINATION

OF STRONTIUM IN WATER
By
Marvin W. Skougstad

Open File Report

Prepared by Quality of Water Branch - October 1957

S?-Un..
• CONTENTS

Page
Objective of present project ••••••..••••••••••••••••••••••••• 1
Introd.uction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . • . . . 1
Equiprilent . • . . . . . . . • . • • . . . . . . . . . . . • . . . . . . • • . . . . . • . . . . • . • • . . • • . 1
Experiment l. Calibration of solutions of NaCl, KCl,
SrCl2 and CaCl2 ...... , ~ . . . . . . . . . . . . . . . . . • . . . . . . . . . . . 2
Experiment 2. The effect of added Na on Sr emission
( 461 mu) . . . . . . . . . . . . . . . . . . . . . . • . . . . . . . . . . . . • . • • . . . . . 3
Experiment 3. The effect of added Ca on Sr emission
at 461 mu . . . . . . . . . . • . . . . . . • • . . . • • • . • . • . . • . . . . • • • • • • 5
Experiment 4. The effect of added KCl on emission of
Sr at 461 mu . . . . . . . . . . . . . . . . . • . . . . . . . . . . . . . • • . . . . . • 5
Analysis of water sam.ples . . . . . . . . . . . . . . . . . . . . . . . . • . . • . . . • . . . . 9

ILLUSTRATIONS

Figure 1. Calibration curve for sodium...................... 4

2. Calibration curve for potassium.................... 5
3. Calibration curve for strontium................... 6
4. Calibration curve for calcium..................... 7
5· Effect of added sodium on strontium emission
( 461 mu) . . . . . . . . . . . . . . . . . . . . . . . . . . . • . . . • . . . . . . . . 9
6. Effect of added calcium on strontium emission
( 461 mu) . . . • . . . . . . . . . . . . . . . . . . . . . . . . . . • . • . . • . . . . 11
7· Effect of added potassium chloride on strontium
emission ( 461 mu). . . . . . . . . . . . . . . . . . • . . . . . . . . . . . . • 13
8. Calibration curve for strontium •••.••••••••••••••• 14

TABLES

Table l. Operating conditions for calibration data ••••••••· 3

2. Effect of added sodium on strontium emissi:•n
( 461 mu) . . . . . . . • • . . . . . . . . . . . . . • • . . . . . . . . . • • • • • • . 8
3. Effect of added sodium on strontium emission
( 680 mu) . . . . . . . . . . . • . . . • . . . . • . . . . • • • . • . . • . . . • • • • 8
4. Effect of added calcium on strontium emission
( 461 mu) . . • . . . . . . . • . . . . . . . . . . . • • . . • . • • . . . • . • . • . • 10 .
5· Effect of added potassium chloride on strontium
emission ( 461 mu) , . . . . . . . . . • . . . . . . . . . . • . . . . . • . . . 12
6. Calibration data for strontium ••••••••••.•.••••••• 12

I
 Page
Table 7· Effect of calcium on strontium determination •••••••• 15
8. Effect of large amounts of calcium on strontium
determination . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . • . . . . 15
9· Effect of various substances on strontium
detei'Dli.nation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . • . 16

II
.
FLAME PHOTOMm'RIC DETERMINATION OF
STRONTIUM IN WATER

By
•
Marvin W. Skougs tad !J

OBJECTIVE OF PRESENT PROJECT

The objective of the present project has been to develop a

procedure for the flame photometric determination of Sr in natural
water samples, utilizing the Beckman Modf' l DU spectrophotometer with
flame photometer attachment, the oxygen-hydrogen flame, and a photo-
multiplier tube attachment. Of special concern was the determination
of Sr at relatively low concentrations, i.e. 0 to 50 ppm.

INTRODUCTION

Preliminary search of reported methods of Sr analysis revealed

several investigations which have been made for the determination of
Sr witt the flame photometer, both at relatively low concentrations
( 0 to 50 ppm Sr) and at higher concentrations. Generally the proc~durea
described involved measurement of Sr emission at either 46o.7 mu or at
681 mu. There is disagreement among thos~ reporting methods for Sr as
to the preference of the one wavelength over the other. The 681 line
(or band) seems to be preferred because of its greater reproducibility
and relative freedom from interference. The 46o.7 mu line, however,
lies in the region of greater sensitivity of the photomultiplier tube,
and hence for this reason is preferred by some. This is an advantage,
of course, when determining Sr at very low concentrations.

This investigation is concerned with determining the optimum

conditions for the determination of Sr at low concentration levels in
water samples. Early experimental work indicated a greater sensitivity
for the 46o.7 mu (hereafter designated as 461 mu) Sr line. Therefore,
most of the subsequent work was based on a study of the effects of
various other materials and conditions on the emission of Sr at this
wavelength.

EQUHMENT

The instrument used for this investigation was the Beckman

Model DU spectrophotometer with a Beckman flame photometer attachment.
The flame photometer consists of a small atomizer-burner which sprays the
sample directly into an oxygen-acetylene flame. The manufacturer's
recommendations state that optimum efficiency is obtained when the

!/ A summary report of a research project carried out on a part-time

basis, St. Olaf College, Northfield, Minn., September 1956 to
May 1957·
1
. 2

atomizer-burner is operated at an oxygen pressure of 10 lb.jsq. in.

By observation of the flame while varying the oxygen pressure, it was
concluded that this pressure does give the most satisfactory flame as
far as size, shape, and stability are concerned. Further testing
showed that the optimum pressure for acetylene lies between 5.0 and
6.0 lb./sq. in. At acetylene pressures less than 5.0 lb./sq. in. the
emission intensity drops off rapidly due to the decrease in flame
temperature. At pressures above 6.0 lb./sq. in. the stability of the
flame was grea·~ 1_y decreased and rapid, more or less erratic fluctuations
in emission intensity were observed. Optimum operating conditions were
thus established at 10 lb.jsq. in. oxygen pressure, and at either 5.0,
5.5, or 6.0 lb./sq. in. acetylene pressure.

The photomultiplier attac ~ment is the standard unit supplied by

Beckman Instruments, Inc., and consists of an auxiliary battery box, con-
taining the necessary "C" batteries, and a special phototube housing
with a special 1P28 multiplier tube. The resistor box, mounted on the
phototube housing, is equipped with a 22 megohm load resistor for
operation with the photomultiplier tube. A red-sensitive phototube and
two additional load resistors (2,000 megohm and 10,000 megohms) mounted
in the phototube housing and resistor box permit the instrument to be
operated as a spectrophotometer or flame photometer over a wide range
• of wavelengths and sensitivities •

Sensitivity of the photomultiplier tube was adjusted by varying

the potential applied to the tube. This was done by eliminating one or
more of the "C" batteries supplying the high voltage to the tube, thus
decreasing the sensitivity of the tube. In most cases the photomultiplier
tube was operated at full sensitivity. Excellent stability and freedom
from fluctuations and drift was attained.

Experiment 1 ••• Calibration of Solutions of NaCJ, KCJ, SrCl2 and CaCl2.

To test the operation of the instrument and particularly the photo-
multiplier attachment which was installed specifically for this investi-
gation, calibration curves were run on solutions containing a single
salt: NaCl, KCl, SrCl2 or CaCl2.

A stock solution of NaCl and of KCl was prepared by drying

reagent grade salt for several hours at 110°, weighing carefUlly the
calculated amount of reagent, transferring the weighed amount quanti-
tatively to a volumetric flask, and diluting to exact volume with
distilled water. Usually 500 ml of stock solution was prepared,
requiring about 1.27 g of NaCl and about 1.00 g of KCl to prepare a
solution of about 1000 ppm of the cation. The exact concentration of
the metal ion was calculated in each case. Aliquots of the stock
solution were diluted to 100 ml in volumetric flasks in order to prepare
standard solutions varying in concentration from 0 to 100 ppm or more as
desired.

Stock solutions of Sr and Ca (chlorides) were prepared by

carefUlly weighing thoroughly di _·· ~d, reagent quality SrC03 and CaC03
 3
•

and transferring the weighed salt to a volumetric flask. Dilute (l~)

HCl was then added in smaJ.l portions until the sample was completely
dissolved. The solution was then diluted to exact volume •
•
All stock solutions and any diluted standard solutions were
transferred immediately after preparation to polyethylene bottles for
storage.

Figures 1, 2, 3, and 4 show typical calibration curves

obtained for NaCl, KCl, SrCl2 and CaCl2 solutions respectively. The
operating data is shown in table 1.

Table 1 ••. Operating conditions for calibration data

Solution NaCl KCl CaCl2 SrCl2

Oxygen, lb./sq. in. 10 10 10 10
Acetylene, lb./sq. in. 6.0 5·0 5.0 5·0
Wavelength, mu 589 770 422 461
Phototube .EM Red .EM .EM
Load resistor, megohms 22 10,000 22 22

• Experiment 2 ••• The effect of added Na on Sr emission 461 mu A series

of standard solutions were prepared, each containing 13. ppm of Sr. To
each was added varying amounts of Na (NaCl standard solution) up to 105
ppm of Na.

Whereas Na alone showed no emission at 461 mu (Sr), the addition

of NaCl to strontium solutions increases the intensity of the Sr emission.
See table 2 and figure 5· Backgrounu intensity measured at 459 mu is
included for comparison. These data indicate that the presence of even
10 ppm of Na (as NaCl) Will cause an error in measurement of Sr at 461 mu.

The effect of the p~esence of Na on Sr emission at 68o mu was

also measured. The effect was not as great at this longer wavelength
as at 461 mu, but because of the much decreased sensitivity of the
photomultiplier unit at these wavelenghts, no further tests were made.
The data in table 3 illustrate the effects observed.
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Table 2 .•• Effect of added Na on Sr emission (461 mu)

Operating data: 10 lb Oxygen, 6.0 lb Acetylene, PM tube,

22 megohm resistor

Concentration of Relative intensity

solution, ppm at wavelength
461 mu 459 mu
Na Sr

o.o o. 0 4.4 4.5

o.o 13.4 38.0 4.5
10.5 13.4 42.2 4.5
21 13.4 45.6 4.5
31 13.4 47-9 4.8
42 13.4 50.1 4.6
63 13.4 53.2 4.6
105 13.4 56.0 4.7

3-1 o.o 4.4 4.3

13.1 0.0 4.4 4.6
26.2 o.o 4.4 4.6
52.4 o.o 4.4 4.6

Table 3 .•• Effect of added Na on Sr emission (680 mu)

Concentration of solution, Relative intensity at

ppm 68o mu
Na Sr

o.o 0.0 2.0

o.o 13.4 5·5
10.5 13.4 6.0
21 13.4 6.3
31 13.4 6.8
42 13.4 7-0
63 13.4 7.2
105 13.4 7.6
3.1 0.0 1.9
13.1 o.o 2.0
26.2 o.o 2.1
52.4 o.o 2.2

Operating data: 10 lb Oxygen, 6.0 lb Acetylene, PM tube,

22 megohm resistor

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 10

~eriment 3 ••• The effect of added Ca (CaCl2) on Sr emission at

1 mu. A series of standard solutions were prepared, each containing
• 13.4 ppm of Sr. To each was added varying amounts of Ca (CaCl2 standard
solution) up to 100 ppm Ca.

Previously, solutions containing up to 200 ppm Ca alone had

shown little or no emission interference at 461 m~ (Sr). 950 ppm Ca
showed significant interference at 461 mu (Sr). The additi on of Ca
increased slightly the intensity of Sr emission above that which would
have b~en expected as due to Ca emission alone. Table 4 and figure 6
shows the data obtained.

Table 4 ••• Effect of added Ca on Sr emission (461 mu)

Concentration of solution Relative intensity at wavelength

ppm Ca ppm Sr 423 mu 461 mu
o.o o.o 3·5 4.3
0.0 13.4 3.6 20.3
9·5 13.4 21.2 22.1
19.1 13.4 38.3 23.5
28.6 13.4 62.0 24.8
)8.1 13.4 61.1 26.1
57.2 13.4 93.0 27.4
76.2 13.4 28.1
95·3 13. 4 off scale 29.1

E!Periment 4 ••• The effect of added KCl on emission of Sr at 461 mu.

A series of standard solutions were prepared each containing 13.1
ppm of Sr. To each was added varying amounts of solid, reagent quality
KCl.

The addition of a large excess of solid KCl increased the

intensity of 461 mu (Sr) and also increased the intensity of background
radiation measured at 459 mu. Also, it was found that the addition of
solid KCl beyond a certain minimum tended to increase the intensity of
emission at 461 mu (Sr) proportionally less, and that the ratio of 461 mu
(Sr) to459 (background) remained essentiaLly constant. This is shown by
the data in table 5 and also in graph 7 •

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Table 5··· Effect of added KCl on Sr emission {461 mu}
.J

Added KCl, Relative intensity at

g/100 ml 461 mu 459 mu
o.o 36 8 (Note) All solutions con-
0.5 67 11 tained 13.1 ppm Sr.
1.0 72 14
2.0 80 25
4.0 85 29
8.0 109 50

A calibration curve was then prepared from a series of standard

Sr solutions containing from 0.0 to 39.2 ppm Sr, and each containing 1.0 g
of solid KCl per 100 ml of standard solution. The data are shown in
table 6 and the data graphed in figure 8.

Table 6 ••• Calibration data, Sr

Concentration Relative intensity Difference

Sr, ppm 461 mu 459 mu (461 - 459)
o.o 10.6 10.6 o.o
2.6 18.4 9·5 8.9
5.2 28.0 9.8 18.2
;.
13.1 54.3 9.0 45.3
19.6 74.0 9.0 65.0
26.1 97·3 9·9 87.4
All samples contained 1.0 g KCl added per 100 ml.

Solutions containing 19.6 ppm Sr and Ca added up to 500 ppm

of Ca. The data obtained (see table 7) showed that the added Ca had
no direct effect on Sr determinat1on when the background reading at
459 mu was subtracted from Sr emission at 461 mu. The errors are
small, are completel y random, and do not indicate any relationship
between increased amounts of Ca and the determination of Sr.

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Table 7 ••• Effect of Ca on Sr determination
.l
Concentration Ca, Relative intensity Concentration Sr, ppm
ppm 461 mu 459 mu Added Found

o.o 85 10.3 19.6 22.0

10.2 82 10.3 19.6 21.5
20.5 82 10.3 19.6 21.5
51.2 79 10.9 19.6 20.0
102 79 10.6 19.6 20.0
205 8o 10.7 19.6 20.5
512 84 11.6 19.6 21.5

Solid CaCl2.2H20 in large excess vas added to a series of

standard Sr solutions, each containing 19.6 ppm Sr. It was found the
Ca concentration could be increased to 5000 ppm Ca without significantly
affecting the Sr determination. The results are tabulated in table 8.

Table 8 ••• Effect of large amounts of Ca, Sr determination

Concentration Relative intensity Concentration Sr, ppm
Ca, ppm 461 mu 459 mu Added Found
&

... o.o 72 10 19.6 18.4

100 67 10 19.6 16.8
• 200 67 10 19.6 16.8
500 70 11 19.6 17.6
• 1000 72 12 19.6 17-7
2000 70 11 19.6 17.6
5000 78 18 19.6 17.7

A series was also run using solid K~Os instead of KCl as the
added radiation buffer. Such solutions required additional acid to be
added in order to prevent precipitation of CaCOs and other insoluble
carbonates. The pH of these solutions therefore varied from a bout
pH = 11 for those containing no Ca, to pH = 3fbr those containing
• 500 ppm and more Ca. No consistent measurements of Sr emission
could be obtained under these conditions. However, the alkaline
solutions seemed to give the best results. The use of K2904 as a
radiation buffer did not improve conditions.

Several types ot materials were tried ao additives, including

NaCl, Fe(NH4)2(S04)2, euso., Na~o.,
and Sodium Versenate. Quite erratic
all cases. At any rate, it appeared
of KCl as the additive.
••
Tartaric Acid, NH4SCN 1 K2Al2(S04)4,
results were obtained in nearl7
preferable to stay with the uoe
• 16

••
Satisfactory results were obtained when solid KCl was added
in the ratio of 1.0 g of solid KCl per 100 ml of solution, and 0.5 g of
ammonium citrate added per 100 ml of solution. The solution is then
made alkaline to phenolphthalein with solid, reagent grade KOH. This
procedure was tested with a limited number of possible interfering
substances. For example, 1000 ppm of 804 and 460 ppm of Na did not
interfere with the Sr determination. In all cases it is necessary to
subtract the background reading at 459 mu from the intensity of the
emission of Sr at 461 mu.

Time has not permitted complete and exact determination of the

extent of interferences due to the presence of various materials in
solution. Interferences were determined in an approximate way, on a
"Go" or "No-go" basis by adding a considerable amount of various salts
to samples of standard Sr solutions, and measuring the 461 to 459
intensity difference. The results, as shown in table 9, indicate that
this technique is probably acceptable for the determination of Sr in
the presence of significant amounts of other dissolved materials.

It should be pointed out that the KA1(S04 ) 2 practically

eliminated Sr emission at 461 mu. Also, the Fe(NH 4 ) 2 (S04 ) 2, when
' present in fairly large amounts, depressed the Sr emission appreciably
and would cause significant error.

Table 9··· Effect of various substances on Sr determination

' Material added Amount Relative intensity ppm Sr
461 mu 459 mu Added Found

2.8 g/1 44.0 19-3 7.8 5·7

II
1.4 g/1 47.4 17.2 ?.8 7-1
II
0.3 g/1 48.2 16.8 7.8 7.8
, CaCl2.2H~ 1.8 g/1 51.3 17.8 7.8 7-9
A1K(S04)2.l2H20 3.8 g/1 19.0 17.2 7.8 0.3
Na~03 2.8 g/1 51.0 18.4 7.8 7.6
Na~03 + NaCl 3.2 g/1 51.0 19.4 7.8 7.4

A concentration of 2.8 g of ferrous ammonium sulfate per liter

corresponds to an iron concentration of about 375 ppm. The addition of
ferrous ammonium sulfate at a concentration of 0.3 g per liter (about
40 ppm Fe) did not cause any error in the Sr determination.

This procedure should be tested completely for the exact' extent

• of interference by substances likely to be encountered in regular w~ter
analysis applications.
.'
t
• 17

• The procedure finally established as giving the most reliable

results for Sr determination is as follows:

1. Add about 50 ml of the sample to be analyzed to a 100 ml

volumetric flask or calibrated bottle.

2. Add 1.0 of high purity solid KCl and 0.5 g of reagent

quality Ammonium Citrate to the sample in the flask.

3. Add three drops of phenolphthalein indicator to the sample,

shake to dissolve all KCl and Ammonium Citrate added and to
thoroughly mix the sample.

4. If the solution is not alkaline (pink) add solid KOH until

a definite pink color is apparent.

5· Mee~ure the relative intensities of Sr (461 mu) and

background (459 mu) with the flame photometer.

The following settings were standardized for all flame photo-

meter measurements:

Oxygen pressure: 10 lb./sq. in.

• Acetylene pressure: 5·5 lb./sq. in •
• Slit width: Not determinable on our instrument as the scale has
been shifted so that the slit width readings have
no meaning. However, the slit width employed was
always very small, as indicated by the sharpness of
the line measured, and the extreme difference in
intensity readings obtained over a very short wave-
length span.
Sr line wavelength: 461 mu.
Background wavelength selected: 459 mu.
Photomultiplier phototube at full sensitivity.
Load resistor: 22 megohms.

ANALYSIS OF WATER SAMPLES

•
Three samples supplied by Mr. c. S. Howard of the Menlo Park
laboratory were analyzed for Sr. These samples contained high concen-
trations of sodium, chloride, and bicarbonate, and, in one sample,
sulfate also. The analysis attempt was made in the middle of our
attempts to establish a standard procedure and so were not considered to
be entirely reliable. The three samples showed some Sr present by .the
method used, but the results did not agree with analysis resu1ts previously
• reported.

.' Sample No.

1
MWS

0.9 ppm
Previously Reported
A
12 ppm
B
20 ppm
2 0.6 " 3.8 " 3.8 II

3 0.1 u 0 11
 18
•
Five samples were submitted by Mr. John Hem of the Denver
• Laboratory. Although results of chemical analysis of the ~ e samples
were not furnished, the data on specific conductance, which was supplied,
indicated a much lower total dissolved solids content in these samples
than in the California samples. These samples were analyzed for Sr.
Only one of the five samples showed a detectable amount of Sr (about
0.2 ppm). It is reasonable to expect that the results of this analysis
are reliable •

•
••

.'