Professional Documents
Culture Documents
Supermini200
MAIN POINTS OF LIQUID ANALYSIS METHODS
RIGAKU CORPORATION
ME1A-74 20161118
Main Point of Liquid Analysis Methods
CONTENTS
1. OUTLINE ..................................................................................................... 1
1. OUTLINE
One of the features of the X-ray fluorescence analysis is that it is possible to measure liquid,
solid and powder samples rapidly as they are. Unlike a solid or powder sample, a liquid
sample is generally measured with the sample chamber kept in the helium atmosphere. A
sample protection film made of polypropylene, Mylar or the like is stuck on a dedicated
liquid sample cell, and solution is poured in it for a measurement.
When an analysis is made using the liquid method, a sample protection film may be torn,
solution in a cell may scatter and a serious accident to the instrument may occur. Factors of
the breakage of a sample protection film are as follows:
Concerning Factor (1), the chemical resistance of a sample protection film against a
sample to be analyzed must be investigated.
Concerning factors (2) and (3), the load (kV-mA) of the X-ray tube must be reduced,
a measurement time must be shortened and a thicker sample protection film must
be used.
Since the basic knowledge of solution is also very important information, sufficient care
must be taken when analyzing a completely unknown sample.
This manual describes methods to measure liquid samples using the Supermini200 and
precautions concerning measurements.
Cat.No. Name
Put a center ring in a helium sample holder, and then put a sample cell. If the film
protrudes from the top of the holder by 5mm or more, cut it using scissors or the like.
Center Ring
Although only the roll type is shown above, films that have been cut into rectangles and
circles are also available. For details, see the catalog “SAMPLE PREPARATION
INSTRUMENTS AND ACCESSORIES FOR X-RAY FLUORESCENCE ANALYSIS”.
Cu Ti Ca Cl P Si Al Mg Na F (KA)
1 ① 1.5μ m Ultra-polyester
ウルトラポリエステル (CH090)
(CH090)
② 4.0μ m Prolene
プロレン (CH416)
(CH416)
③ 6.0μ m Polypropylene
ポリプロピレン (RS1440-P)
(CH425)
0.8 ⑩12.0μ mMylar
ポリプロピレン(CH475)
(CH150)
⑨ 5.0μ m Polypropylene (CH475)
マイラー (RS1440-F)
④ 6.0μ m Mylar
マイラー(CH250)
(CH250)
Transmittance
⑦ 7.5μ m Kapton
キャプトン(CH442)
0.6
(CH442)
透過率
0.4
0.2
0
0 5 10 15 20
波長(A)(A)
Wavelength
N: Not contained at all, V: Very small quantity contained, S: Small quantity contained,
C: Contained, L: Large quantity contained
Data reduction has been made by referring to data obtained by measuring 10 films
placed one upon another using a hollow Ti cup. For impurity lines generated from
the optical system etc., make an investigation by measuring a blank sample.
5
6
10
11
12
Transmittance varies depending on a sample protection film used. For example, when
a Mylar film with a thickness of 6m is used, it is probably impossible to obtain useful
data from the measurements of F and Na because transmittance for them becomes
almost zero. In this case, delete “F-KA” and “Na-KA” for the qualitative analysis. For
deletion, right-click an element to be deleted to make the button for deletion displayed,
and click it.
The fixed time measurement is a function to carry out fixed time counting for a
specified component at peak and background angles and makes it possible to obtain
X-ray intensities with smaller statistical errors of counting. It is very effective to analyze
trace components.
1 2
Available Films
When a protection film is stuck, sensitivity for light elements decreases as the
graph in Section 3.1 shows. Therefore, be sure to set correctly the sample film to
be used. The sample film absorption correction is made according to the sample
film that is set here.
When diluent is set, analysis values are calculated with X-ray absorption by the
diluent taken into consideration.
5 6
Library
Step
The tube voltage and current are fixed to 50kV and 4mA respectively.
The X-ray tube load (kW) is calculated as follows:
kW = kV mA / 1000
Be sure to check a time necessary for a sequence by actually measuring a cell filled
with water using the prepared qualitative application condition.
5. EXAMPLES OF MEASUREMENTS
OF STRONG ACID SOLUTIONS
If a sample protection film is torn, acid solution will cause serious damage to an instrument.
The handling and measurement method especially of strong acid solutions are described
below. As already described, basically it is important to make a measurement in a short
time.
The table below shows the result of the resistance test that is known visually from the
photographs.
Result of Resistance Test for Sample Protection Films Against Strong Acids
Polypropylene Kapton Mylar (Polyester)
Aqua Regia G G F
Concentrated Nitric Acid G F N
Concentrated Hydrochloric Acid G G F
G: No change was found with the film. F: A small swell was found with the film. N: A
swell and a leak were found.
The result is almost the same as that in the table of the typical chemical resistance and X-ray
resistance of high polymer films in Section 3.2.
From the above result, it is presumed that polypropylene films are useful for strong acid
solutions. A small number of bubbles were produced in the case of aqua regia and every film,
but they were produced after some time passed, not immediately after aqua regia was poured
into a cell.
Accessories to Be Used
Specification of
Cat.No. Name
Accessory
3399O252 (RS6020) Thin Film Assembling Jig for liquid Ball, Pipe
(1) Put the ball on the tube (2) Lay a thin film lightly (3) Put the snap-on ring on the thin film
laid in Step (2), and set the thin film
and cover them with the and hold it using the ring to the cell. In this step, set the ring
polyethylene sample cell of the thin film fixing jig by hand. Now the side other than the
analysis side has been prepared.
(4) After turning the cell upside down and pouring analysis (5) Now the sample preparation has
sample (solution) into the cell, stretch a film on the
analysis side using the thin film fixing jig. This work can been completed.
be done easily by setting the film after putting the ball of
the thin film assembling jig for liquid on the base in the
lower part of the thin film fixing jig.
When X-rays irradiate liquid sample, its temperature rises and pressure in a sample
cell increases. This increase in the pressure can be reduced and the sample can be
sealed in the cell by stretching a thin film loosely using these jigs on the other side of
the polyethylene sample cell than the analysis side.
Measuring Time
Since sample cannot be sealed perfectly even when it is prepared according to the
procedure described in Section 5.2, a very small quantity of a volatile substance will
leak into the instrument and cause the corrosion of its inside if the sample contains a
large quantity of the volatile substance. Therefore, decrease the number of elements
to be measured using one sample, and make a measuring time as short as possible.
After Measurement
6. SUPPLEMENT TO CAUTIONS
CONCERNING SOLUTION
ANALYSIS
Described below is a supplement to the cautions concerning solution analysis, though some
parts may overlap with the contents on the previous pages.
Kapton and Mylar are registered trademarks of Du Pont of the United States.
Prolene, Ultra-Polyester and Etnom are trademarks of Chemplex of the United States.
<Blank Page>