JP2000292318A - High-speed collecting method of sample and high-speed diluting device using it - Google Patents

Abstract

PROBLEM TO BE SOLVED: To stably supply a sample at low speed without deteriorating the throughput by introducing the sample at high speed by a high-speed feed pump, partially branching it by a splitter, and slowly supplying it at a constant flow rate to an analyzing device by a low-speed feed pump. SOLUTION: A large quantity of a sample collected by an auto sampler 20 is fed by a high-speed feed pump 22 at high speed, and mixed with a diluting solution 14 in a combiner 26 to form a turbulent flow, which is then partially branched by a splitter 30, and the branched sample is slowly sent to a nebulizer 36 at a constant flow rate by a low-speed feed pump 32 to stabilize the output signal. The sample sent to the nebulizer 36 is atomized, and guided to a plasma touch 50 after removing the drain by a spray chamber 38. The drain discharge through the drain port 39 of the spray drain chamber 38 is slowly guided to a drain tank 44 at a constant flow rate by a drain discharge pump.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a high-speed sampling method for a sample and a high-speed dilution apparatus using the same, and more particularly, to a method for atomizing a sample solution such as a high-frequency inductively coupled plasma mass spectrometer (ICP-MS). A high-speed sample collection method suitable for use when introducing a sample into an analyzer having a nebulizer to be converted, capable of stably supplying a sample at a low speed without deteriorating throughput, and a method for using the same. High-speed dilution device.

[0002]

2. Description of the Related Art In an analyzer such as an ICP-MS having a nebulizer, it is necessary to supply a sample stably at a low speed.

Therefore, conventionally, US Pat.
As described in the specification of Japanese Patent No. 7, for example, a sample is sent using one pump, and the rotation of the pump is adjusted so that the sample sending speed decreases when the sample reaches the nebulizer. There is a program control method.

[0004]

However, there is a problem that the distance from the autosampler for automatically collecting a sample to the nebulizer is long and the throughput is low.

When the pumping speed is increased in order to improve the throughput, the load on the plasma generated by the subsequent plasma torch becomes large because only one pump is used. An interface nozzle for sampling an ionized element under atmospheric pressure and introducing it into an ion lens under vacuum, a plasma (for example, an IC)
There is a risk that the plasma torch for generating P) may be clogged. If a method is adopted in which the liquid sending speed is reduced when the sample sent reaches the nebulizer, the plasma becomes unstable due to a sudden change in the flow rate. Problems.

In US Pat. No. 5,646,727, it is described that a pump for sending an internal standard substance is provided in addition to a sample sending pump. And did not make it possible to send a large amount of sample.

The present invention has been made to solve the above-mentioned conventional problems, and has as its object to stably supply a sample at a low speed without deteriorating the throughput and stabilize an output signal of an analyzer or the like. And

[0008]

According to the present invention, when a sample is collected at a high speed, the sample from the autosampler is introduced at a high speed by a high-speed liquid sending pump, and after being partially branched by a splitter, it is fixed by a low-speed liquid sending pump. This problem is solved by slowly sending the sample to the analyzer at a flow rate.

Further, a diluent introduced by a diluent introduction pump is added to the sample by a mixer provided between the high-speed liquid sending pump and the splitter to dilute the sample.

Furthermore, a turbulent flow is generated in the preceding stage of the mixer by a combiner having a V-shaped groove therein to ensure mixing of the sample and the diluent.

Further, the internal standard substance is also sent to the ground combiner provided in the preceding stage of the analyzer by the low-speed liquid sending pump, so that the internal standard substance can be easily added online.

Further, the ground combiner is grounded,
This excludes the effects of static electricity.

In addition, the internal standard substance is supplied by the high-speed liquid supply pump or the diluent introduction pump so that these abnormalities (sets, consumption, etc.) can be diagnosed.

The present invention also provides a high-speed sample diluting apparatus, a high-speed liquid feed pump for introducing a sample from an autosampler at a high speed, a diluent liquid introducing pump for introducing a diluent, and the high-speed liquid feeding pump. A mixer for mixing the sample introduced by the liquid pump and the diluent introduced by the diluent introduction pump, a splitter for branching a part of the sample diluted by the mixer, and a splitter for splitting by the splitter. This problem is solved by providing a low-speed liquid feed pump for slowly feeding the sample at a constant flow rate to the analyzer.

[0015]

Embodiments of the present invention will be described below in detail with reference to the drawings.

The first embodiment of the high-speed diluting apparatus according to the present invention for performing high-speed sampling of a sample and diluting the sample with a diluent, as shown in FIG. An autosampler 20 for automatically sampling the washing liquid 12 for washing at the time of non-analysis, a high-speed liquid sending pump 22 for introducing a sample collected by the autosampler 20 at a high speed, and diluting the sample 10 A diluent introduction pump 24 for introducing the diluent 14, and a turbulent flow in the sample 10 and the diluent 14 introduced from the high-speed liquid supply pump 22 and the diluent introduction pump 24 to ensure mixing. A combiner 26 having a V-shaped groove therein, a mixer 28 for mixing the sample 10 and the diluent 14 turbulently generated by the combiner 26, and a mixer 28 A splitter 30 for branching a part of the sample, and a low speed for slowly sending the sample branched by the splitter 30 and the internal standard substance (ISTD) 16 to the nebulizer 36 of the ICP-MS at a constant flow rate. A liquid feed pump 32, a ground combiner 34 whose body is grounded for mixing the sample sent by the low-speed liquid feed pump 32 with the internal standard substance, and a drain hole 39 of a spray chamber 38 downstream of the nebulizer 36. And a drain discharge pump 42 for slowly guiding the drain removed from the drain tank 44 to the drain tank 44 at the same speed as the low-speed liquid feed pump 32.

The high-speed liquid supply pump 22, the diluent introduction pump 24, the low-speed liquid supply pump 32, and the drain discharge pump 42 include, for example, a flexible tube T as described in US Pat. No. 5,646,727. A roller R rotated by a rotating drum D and a pressure plate P
Can be used.

The flow rate of the high-speed liquid pump 22 may be higher than that of the low-speed liquid pump 32.

The ratio between the flow rate of the high-speed liquid sending pump 22 and the flow rate of the diluent introducing pump 24 is the dilution ratio of the sample.

The rotation and driving operation of each pump is program-controlled, and the whole pump automatically moves.

The nebulizer 36 can be of any type, such as a cross-flow type or a V-groove type. The inner diameter of the pipe is not limited.

The operation of the first embodiment will be described below.

The sample collected by the autosampler 20 is
After a large amount of liquid is sent at high speed by the high-speed liquid sending pump 22 and mixed with the diluent 14 by the combiner 26 to form a turbulent flow,
The mixture is mixed by the mixer 28, then partially branched by the splitter 30, and the branched sample is slowly sent to the nebulizer 36 at a constant flow rate by the low-speed liquid sending pump 32, thereby stabilizing the output signal.

The sample sent to the nebulizer 36 is atomized, and after the drain is removed in the spray chamber 38, the sample is guided to the plasma torch 40. The drain discharged from the drain hole 39 of the spray chamber 38 is slowly guided to a drain tank 44 at a constant flow rate by a drain discharge pump 42.

In this manner, the sample sent at a relatively large flow rate by the high-speed liquid sending pump 22 is partially branched by the splitter 30, and the branched sample is separated by the low-speed liquid sending pump 32 at a relatively small constant flow rate. By sending the plasma to the nebulizer 36, a stable plasma can be formed without lowering the throughput.

In the present embodiment, the ISTD 16 is also supplied by the low-speed liquid supply pump 32 and is supplied to the ground combiner 34.
The ISTD can be added without interrupting the supply of the sample to the nebulizer 36. In addition, the flexible tube T for sending the sample by the low-speed liquid sending pump 32 is used.
By appropriately selecting the inner diameter of s and the inner diameter of the flexible tube Ti for sending ISTD,
The amount of D added can be determined.

In the present embodiment, since the body of the ground combiner 34 is grounded, the influence of static electricity can be eliminated.

It should be noted that, as with the low-speed liquid supply pump 32,
The TD 16 is supplied with a high-speed liquid supply pump 22 or a diluent liquid introduction pump 24.
, It is possible to diagnose abnormalities such as settling of the high-speed liquid sending pump 22 and the diluting liquid introducing pump 24 and the degree of consumption.

Next, a second embodiment of the present invention will be described in detail with reference to FIG.

This embodiment uses an internal standard substance other than the sample (dilution ratio internal standard substance) for accurately obtaining a dilution ratio (dilution ratio) in the same high-speed dilution apparatus as the first embodiment.
DFIS) 18 can be supplied to the combiner 26 by the high-speed liquid supply pump 22.

The other points are the same as those of the first embodiment, and the description is omitted.

According to the present embodiment, the dilution ratio can be accurately obtained by using the DFIS 18.

[0033]

EXAMPLE FIG. 3 shows data obtained by examining the reproducibility of the dilution ratio for 4 hours using the second embodiment. In the figure, "5
"Times", "10 times" and "20 times" are 5 times and 10 times respectively.
1x, 20x dilution mode (actually due to various errors,
Rh is rhodium, Pd is palladium, DFIS is a dilution ratio internal standard, SMP is a sample, and RSD is a relative standard deviation, respectively.

FIG. 4 shows the sample SMP / dilution ratio internal standard substance DFIS in each dilution mode from the data of FIG.
It is the result of examining the rate of change and examining the rate of change, and it was confirmed that the rate was within a certain range.

In the above description, the present invention relates to an IC
Although used to introduce a sample into a P-MS nebulizer, the application of the present invention is not limited to this.

[0036]

According to the present invention, a sample sent at a relatively large flow rate by a high-speed liquid sending pump is partially branched by a splitter, and the sample is supplied to an analyzer at a relatively small flow rate by a low-speed liquid sending pump. The sample can be supplied stably at low speed without deteriorating the throughput. Therefore, the output signal of an analyzer having a nebulizer such as an ICP-MS is stabilized.

[Brief description of the drawings]

FIG. 1 is a pipeline diagram showing a configuration of a first embodiment of a high-speed dilution device according to the present invention.

FIG. 2 is a pipeline diagram showing the configuration of the second embodiment.

FIG. 3 is a diagram showing data obtained by examining the reproducibility of a dilution ratio according to a second embodiment.

FIG. 4 shows a sample S at each dilution concentration from the data of FIG.
Diagram showing the result of examining the rate of change by determining the ratio of MP / dilution ratio internal standard substance DFIS.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 10 ... Sample (liquid) 12 ... Washing liquid 14 ... Diluent 16 ... Internal standard substance (ISTD) 18 ... Dilution rate internal standard substance (DFIS) 20 ... Autosampler 22 ... High-speed liquid sending pump 24 ... Diluent introduction pump 26 ... Combiner 28 mixer 30 splitter 32 low-speed liquid feed pump 34 ground combiner 36 nebulizer 38 spray chamber 40 plasma torch 42 drain drain pump 44 drain tank

──────────────────────────────────────────────────の Continued on the front page (51) Int.Cl. ⁷ Identification FI FI Theme Court ゛ (Reference) // G01N 21/73 G01N 1/28 T (72) Inventor Shuzo Nagaoka 1-1-15 Nakamachi, Musashino City, Tokyo No. 5 Mitaka Takagi Building Yokogawa Analytical Systems Co., Ltd. (72) Inventor Katsuhiko Kawabata 1-15-5 Nakamachi, Musashino-shi, Tokyo Mitaka Takagi Building Yokogawa Analytical Systems Co., Ltd. F-term (reference) 2G043 AA01 CA03 DA05 EA08 GA07 GB01 GB09 MA01 5C038 EE02 EF01 EF04 GG09 GH05

Claims (7)

[Claims] 1. A high-speed sampling of a sample, wherein a sample from an autosampler is introduced at a high speed by a high-speed liquid sending pump, partially branched by a splitter, and then slowly sent to the analyzer at a constant flow rate by a low-speed liquid sending pump. Method. 2. The method according to claim 1, wherein the diluent introduced by the diluent introduction pump is added to the sample by a mixer provided between the high-speed liquid feed pump and the splitter to dilute the sample. High-speed sample collection method. 3. The method according to claim 2, wherein a turbulent flow occurs in a stage preceding the mixer by a combiner having a V-shaped groove therein. 4. The high-speed sample feeding method according to claim 1, wherein the low-speed liquid sending pump also sends an internal standard substance to a ground combiner provided in a preceding stage of the analyzer. Collection method. 5. The method according to claim 4, wherein the ground combiner is grounded. 6. The high-speed sampling of a sample according to claim 1, wherein the internal standard substance is sent by the high-speed liquid sending pump or the diluent introducing pump, and the abnormality is diagnosed. Method. 7. A high-speed liquid sending pump for introducing a sample from an autosampler at a high speed, a diluting liquid introducing pump for introducing a diluting liquid, a sample introduced by the high-speed liquid sending pump, and the diluting liquid. A mixer for mixing the diluent introduced by the introduction pump, a splitter for branching a part of the sample diluted by the mixer, and a sample branched by the splitter to the analyzer slowly at a constant flow rate. A high-speed sample dilution device, comprising: a low-speed liquid feed pump for feeding.