Turbidimetric Determination of Available Sulfates

LEON CHESNIN and C. H. YiEN2

' I J HE measurement of the sulfate content of soils has Morgan (7) proposed the use of a sodium acetate-acetic acid
•*- received little attention from soil chemists despite buffer solution to extract the sulfate-sulfur content of soil. He
compared the turbidity produced in vials containing the ex-
the fact that sulfur ranks among the essential plant tracts with the intensity of color produced by calcium oxalate
nutrients. Perhaps this has been due in part to the fact precipitates. Morgan pointed out that the test was not sensitive
that the gravimetric method of determining sulfates is over the range of concentrations of sulfate-sulfur present in
time-consuming and requires great care, together with most soils of humid regions, except as a result of heavy appli-
cations of sulfate materials.
the use of an analytical balance. The magnitude of the
errors involved in the gravimetric techniques may even
equal the total amount of sulfate present in a 20-gm EXTRACTION SOLUTION
sample of sandy soil of humid regions. Some of these A comparison was made of the solubility of sulfates in Mor-
sources of error are co-precipitation, losses in the trans- gan's universal extraction solution, which is used in the tur-
fer, or ignition phases of the analysis, as well as con- bidimetric method, with the solubility of sulfates in 0.1 and
densation of moisture on the surface of the crucible dur- 0.5N HQ. After one-half hour of shaking 20 gm of air-dried
Sharpsburg soil in 100 ml of each of the extraction solutions,
ing the weighing of the precipitate. The turbidimetric the suspensions were filtered, washed several times with hot
method of determining sulfates presented in this paper water, and the total amount of the extracted sulfates was pre-
proposes to increase the speed and accuracy of this cipitated with BaCla and determined gravimetrically. This
analysis and permit the measurement of sulfates in process was repeated after adding 0.2 gm of gypsum to the soil
samples prior to the extraction process. The data are presented
volumes of solution which cannot be accomplished by in Table 1. The sodium acetate buffer solution extracted more
the ordinary macro-gravimetric techniques. sulfates from the Sharpsburg soil than did the HQ. solutions.
Hinds (4, 5) determined the sulfate content of water and However, the gypsum added to the soil was more soluble in
urine by measuring the volume of the turbid suspension pro- the acid solutions than in the buffer solution. The recovery of
duced with barium chloride which would obscure the image 102.0 and 98.5% of the sulfur added in the form of gypsum
of a candle flame held under a calibrated tube. Jackson (6) to the 0.1 and 0.5N HQ solutions, respectively, serves to illus-
improved Hind's technique by standardizing the conditions for trate the possible errors in the gravimetric procedure due to
measuring the turbidity of the barium sulfate suspension. He losses of precipitate, and adsorption or co-precipitation of ions.
introduced the use of a standard candle light source, uniform These errors are magnified when the total amount of sulfate
distance, and controlled light . conditions of the background. present is small.
Parr and McClure (8) modified Jackson's apparatus to get
more concentration of light from the candle source.
Denis (2) determined the sulfate content of blood, after the TABLE 1.—Recovery of sulfur added in the jorm of gypsum to
removal of the protein, by comparing the density of the col- 20 grams of a Sharpsburg silty clay loam soil and
loidal barium sulfate to that of a standard. The readings were extracted with 100 ml of solution.
made in a' nephelometer, and no means of dispersing the pre-
cipitate were used. Denis and Reed (3) modified this method
by adding 1 ml of a 5% gelatin solution per 25 ml of barium Recovery
sulfate suspension. The gelatin acted as a protective colloid. Sulfur Sulfur of the
Boutwell and Toepfer (1) determined the sulfur content of Extracting solution in soil added sulfur
urine turbidimetrically by adding sized barium chloride crystals sample to soil added
of 20- to 30-mesh to form the colloidal barium sulfate. The to soil
method was considered to be accurate only in the concentration
range of 20-30 ppm of sulfur. Treon and Crutchfield (10) mgm mgm %
found that if aqueous barium chloride was used instead of 20-
to 30-mesh crystalline barium chloride, the suspension of NaAc buffer. _ 10.3 37.2 83!2
barium sulfate obtained was not lasting, and low and incon- 0 . 1 N HC1 3.4 37.2 102.0
sistent results were obtained. The turbidity readings had to be 0 . 5 N HC1. _ _ _ _ _ _ _ _ _ 8.4 37.2 98.5
made immediately after adding the barium chloride.