Offline pretreatment device and method for simply measuring oxygen stable isotope ratio in water

A stable isotope and water determination technology, applied in measuring devices, material separation, instruments, etc., can solve the problems of differences in measurement results, small reactor capacity, and small amount of sample addition, and achieve low cost, simple operation, and guaranteed determination The effect of precision

Active Publication Date: 2014-08-13
CHINA NAT RES INST OF FOOD & FERMENTATION IND CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the on-line pre-treatment equipment is relatively expensive, the reactor capacity is small, and the amount of sample added is very small. There are literatures that show that the error of the amount of sample added will lead to differences in the measurement results [Research on GasBench II-IRMS Water Equilibrium Hydrogen and Oxygen Isotope Analysis Method], And some part of the reactor is for one-time use, the cost is higher

Method used

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  • Offline pretreatment device and method for simply measuring oxygen stable isotope ratio in water
  • Offline pretreatment device and method for simply measuring oxygen stable isotope ratio in water
  • Offline pretreatment device and method for simply measuring oxygen stable isotope ratio in water

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Combine now figure 1 , figure 2 and image 3 Describe the working process of the device and the analysis and measurement method.

[0045] 1. Add about 4mL of water sample to the reaction bottle (7), and cover it tightly with the cap (with Teflon gasket);

[0046] 2. Connect the reaction bottle (7) to the capillary stainless steel tube (6), open the valve of the carbon dioxide cylinder (1), open the pressure reducing valve (2), and replace the air in the reaction bottle with the upward exhaust method (such as figure 2 ), after 15 minutes, unplug the capillary stainless steel tube (6) from the reaction bottle (7);

[0047] 3. Put the reaction bottle in a water bath at 25±0.2°C, shake it for 10 hours and take it out;

[0048] 4. Set gas chromatography parameters: inlet temperature 100°C, column temperature 100°C, constant flow rate 1.2mL / min;

[0049] 5. Use a gas sampling needle to collect the gas in the reaction bottle (continuous collection by an automatic sample...

Embodiment 2

[0051] According to the method in Example 1, take a certain water sample as the experimental object, process and measure the δ in the water continuously 18 O(n=3), the results are shown in Table 1

[0052] Table 1 Repeated determination of a water sample δ 18 Result of O (‰)

[0053]

[0054] In this example, it has been verified that offline pretreatment device and assay method in the present invention measure δ in water 18 The repeatability of O, as can be seen from Table 1, the 1σ of the present invention is only 0.075‰, which is less than the international standard for water δ 18 Determination requirements of O (0.2‰)

Embodiment 3

[0056] With 4 known δ 18 The water samples of O (see Table 2) were the experimental objects, and the four samples were measured according to the method in Example 1, and the results are shown in Table 2.

[0057] Table 24 kinds of water samples δ 18 o

[0058]

[0059] As can be seen from Table 2, although there is a certain deviation between the measured result and the known value, the analysis data can find that the two are in a good linear relationship, see Figure 4 .

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Abstract

The invention relates to an offline pretreatment device and an offline pretreatment method for simply measuring an oxygen stable isotope ratio in water. The device comprises a carbon dioxide inflation system, a reaction kettle and a constant-temperature oscillation water bath box, wherein the carbon dioxide inflation system comprises a carbon dioxide steel bottle, a pressure reducing valve, a gas inlet branch tube, a rubber pipe and capillary tubes, wherein the pressure reducing valve is connected with the carbon dioxide steel bottle; the gas inlet branch tube is connected with the pressure reducing valve by a connecting guide tube; the rubber tube is connected on the gas inlet branch tube; and the capillary tubes are arranged on the tail end of the rubber tube; one or more, preferably two or more capillary tubes are connected at a sampling branch tube, so that one or more, preferably two or more reaction bottles are connected with the capillary tubes. The method combines an offline pretreatment technology and a gas chromatography-stable isotope ratio mass spectrometer (GC-IRMS) coupling technique, so that precision and accuracy can be ensured. Moreover, the cost is low, a using range of the GC-IRMS is expanded, and using efficiency of the GC-IRMS is improved.

Description

technical field [0001] The invention relates to a method for simply measuring the oxygen stable isotope ratio in water (denoted as δ 18 O) off-line pretreatment device and method, specifically adopt off-line pretreatment technology, utilize gas chromatography-stable isotope ratio mass spectrometry (GC-IRMS) to measure δ in water 18 O, belongs to the technical field of stable isotope determination. Background technique [0002] Oxygen stable isotope in water is an important means for hydrological environment research and food authenticity identification, and popularizing the determination method of oxygen stable isotope in water is also of great significance for food quality supervision and control. [0003] The current determination of δ in water 18 The main method of O is the carbon dioxide-water balance method. The following oxygen isotope exchange is carried out between carbon dioxide and water in a closed reactor (exchange coefficient α=1.0412 at 25°C). After the oxyge...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06G01N30/02
Inventor 钟其顶陈文斌熊正河
Owner CHINA NAT RES INST OF FOOD & FERMENTATION IND CO LTD
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