CN109030704B - Ion chromatograph sample injection volume determination device and sample injection volume determination method - Google Patents
Ion chromatograph sample injection volume determination device and sample injection volume determination method Download PDFInfo
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- G01F—MEASURING VOLUME, VOLUME FLOW, MASS FLOW OR LIQUID LEVEL; METERING BY VOLUME
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Abstract
The invention belongs to a sample injection volume measuring device and a sample injection volume measuring method of an ion chromatograph, belonging to a sample injection volume measuring device and a sample injection volume measuring method of the ion chromatograph, which are used for accurately measuring the sampling volume in full quantitative loop sample injection and partial quantitative loop sample injection of the ion chromatograph. The invention adopts the technical scheme that the sample injection valve is adopted to alternately communicate the inorganic salt solution with the quantitative ring and the flushing liquid with the quantitative ring to the solution passage or the flushing channel, and the sample injection volume measuring device of the ion chromatograph and the sample injection volume measuring method using the device solve the technical problems that the existing sample injection volume calibrating device and sample injection volume calibrating method of the ion chromatograph have low gas flow rate, liquid remains in the quantitative ring, the gas flow rate is high, some liquid can be taken away, the calibrating liquid is easy to evaporate and lose, and the calibrating accuracy is influenced.
Description
Technical Field
The invention belongs to a device and a method for measuring the sample injection volume of an ion chromatograph, in particular to a device and a method for measuring the sample injection volume of the ion chromatograph.
Background
The ion chromatography automatic sample injector is more and more widely applied, has the functions of partial, non-full-circle and sample injection, and greatly improves the use convenience. However, for quantitative loop sampling, especially for non-full loop micro-upgrade sampling, the accuracy of sampling volume is always lacking of a stable and effective detection device and method. The Chinese patent application, application publication No. CN105115561A, a quantitative ring volume verification device and verification method, discloses a quantitative ring volume verification device which comprises a quantitative ring, a six-way valve, a liquid source, a liquid injection pump, a gas source, a gas injection pump, a weighing mechanism and the like, wherein the quantitative ring is connected with the six-way valve, the liquid injection pump, a liquid outlet, the gas injection pump and a gas outlet are respectively connected with one interface of the six-way valve, the liquid injection pump, the quantitative ring and the liquid outlet form a liquid passage, the gas injection pump, the quantitative ring and the gas outlet form a gas passage, the gas passage is communicated with the weighing mechanism, the six-way valve enables the quantitative ring to be switched between the liquid passage and the gas passage, and pushing out the liquid in the quantitative ring by using the gas injected by the gas injection pump, and calculating the liquid volume in the weighing mechanism to obtain the volume of the quantitative ring. In the practice of the device and the verification method, if the air flow purging flow rate is low, liquid can remain in the quantitative ring, and if the air flow purging flow rate is high, some liquid to be detected can be taken away, so that the verification accuracy is influenced; the micro sampling amount needs to be accumulated for multiple times to reach the weighable weight, and the device is in a long-term waiting process, so that the verification liquid is easy to cause evaporation loss, and the verification accuracy is also influenced.
Disclosure of Invention
The invention provides a sample volume determination device and a sample volume determination method for an ion chromatograph, which aim to solve the technical problems that the existing sample volume determination device and sample volume determination method for the ion chromatograph have low gas flow rate, liquid remains in a quantitative ring, the gas flow rate is high, some liquid can be taken away, the loss of the liquid during the determination is easy to evaporate, and the accuracy of the determination is influenced.
In order to solve the technical problems, the invention adopts the technical scheme that: a kind of ion chromatograph advances the volume determination device, including two interfaces of the sample valve of both ends connection of the quantitative loop respectively; a sampling pump conveys the measuring solution into a quantitative ring; the sampling pump is communicated with the interface of the sample injection valve, the quantitative ring and the interface of the sample injection valve to form a solution measuring passage, or the sampling pump is communicated with the interface of the sample injection valve, the quantitative ring and the waste liquid pipe to form a solution measuring passage; the receiving bottle and the weighing mechanism are used for conveying flushing fluid into the quantitative ring by the infusion pump; the infusion pump is communicated with the interface of the sample injection valve, the quantitative ring and the receiving bottle are communicated with the interface of the sample injection valve to form a flushing fluid passage; switching the sample injection valve to a quantitative ring communication measuring solution passage or a quantitative ring communication flushing liquid passage; the measuring solution is an inorganic salt solution with a set concentration, the flushing liquid does not react with the measuring solution (3), and the flushing liquid has no solid solute residue or trace residue in the process of evaporating the flushing liquid and the measuring solution to separate out the inorganic salt, so that the measuring precision is not influenced.
Each end of the quantitative ring is connected with one interface of the sample injection valve. And the sample injection valve is controlled to realize that the conversion quantitative ring is communicated with the solution measuring passage or the conversion quantitative ring is communicated with the flushing fluid passage. Switching a sample injection valve, disconnecting a flushing liquid passage, connecting a measuring solution passage, and enabling the measuring solution conveyed by a sampling pump to enter a quantitative ring; when the sampling pump is in a suction type sampling mode, the sampling pump is communicated with an interface of the sample injection valve, the quantitative ring and a testing solution are communicated with the interface of the sample injection valve to form a testing solution passage; when the sampling pump is in an injection type sampling mode, the sampling pump is communicated with an interface of the sample injection valve, the quantitative ring and the waste liquid pipe are communicated with an interface of the sample injection valve to form a solution measuring passage; switching the injection valve, the disconnection of survey solution passageway, the flush fluid passageway switch-on, interface, ration ring and the interface that the receiving flask intercommunication injection valve of transfer pump intercommunication injection valve form the flush fluid passageway, and the survey solution in the washing fluid washes ration ring, and flush fluid and survey solution get into the receiving flask. Evaporating the washing liquid collected by the receiving bottle and the solvent in the measuring solution, weighing the crystallized salt precipitated from the measuring solution by the weighing mechanism, calculating the weight of the measuring solution according to the weight of the crystallized salt and the set concentration of the salt in the measuring solution, calculating the volume of the measuring solution according to the density of the measuring solution at the temperature during measurement, and accurately obtaining the sample introduction volume according to the volume. The invention adopts the flushing liquid to replace the gas used by the prior quantitative ring volume calibrating device, the flushing liquid flushes the measured solution in the quantitative ring completely, and no residual liquid or loss exists; the determination solution adopts inorganic salt solution with set concentration, no loss is generated in the determination process, the defect of evaporation loss of the determination liquid is eliminated, and the accuracy of the determination result is high. The sample injection volume measuring device of the ion chromatograph is used for measuring the sample injection volume in a full quantitative loop sample injection mode or a partial quantitative loop sample injection mode.
The sample injection valve is a six-way valve, and 1-6 interfaces of the six-way valve are sequentially arranged; the both ends of ration ring are connected 1 interface and 4 interfaces respectively, and the 2 interfaces of injection valve are connected to the transfer pump of being connected with the flush fluid, and the 3 interfaces of injection valve are connected to the receiving flask, and 6 interfaces of injection valve are connected to the sample pump, and 3 5 interfaces of connecting the injection valve are dissolved in the survey. The sample injection valve is switched to the positions of the connection of the interfaces 2 and 3, the connection of the interfaces 1 and 6 and the connection of the interfaces 4 and 5, the flushing liquid, the infusion pump and the receiving bottle are not communicated with the quantitative ring, the passage of the flushing liquid is disconnected, the sampling pump and the determination solution are communicated with the quantitative ring, and the passage of the determination solution is connected; the sample injection valve is switched to the positions of connection of the interfaces 1 and 2, connection of the interfaces 3 and 4 and connection of the interfaces 5 and 6, the sampling pump and the determination solution are not communicated with the quantitative ring, the passage of the determination solution is disconnected, the flushing liquid, the infusion pump and the receiving bottle are communicated with the quantitative ring, and the passage of the flushing liquid is connected. This is an aspiration type sampling method in which a sampling pump aspirates a measurement solution into a dosing ring.
The sample injection valve is a six-way valve, and 1-6 interfaces of the six-way valve are sequentially arranged; the both ends of ration ring are connected 1 interface and 4 interfaces respectively, and the 2 interfaces of injection valve are connected to the transfer pump of being connected with the flush fluid, and the 3 interfaces of injection valve are connected to the receiving flask, and 6 interfaces of injection valve are connected to the sampling pump of being connected with survey solution, and 5 interfaces of injection valve are connected to the waste liquid pipe. The method is an injection type sampling mode, firstly, a measuring solution is sucked into a sampling pump, then, the measuring solution is injected into a quantitative ring, and redundant waste liquid is discharged from a waste liquid pipe. The injection sampling mode differs from the suction sampling mode in that the sampling pump adds the measurement solution to the dosing ring in a different manner.
The determination solution is non-toxic and harmless solution, solute salt in the determination solution is selected not to decompose in the process of evaporation of the flushing liquid and the determination solution to separate out crystal salt, and the determination precision is not influenced by no loss or trace loss.
The washing liquid is nontoxic and harmless liquid. The washing liquid with proper evaporation degree is selected, so that the washing liquid can be conveniently matched with the crystal salt evaporated and separated from the solvent in the solution to be measured for use.
When the temperature of the measured solution is 20-30 ℃, the solubility is more than or equal to 30g, and the boiling point is less than or equal to 150 ℃. The solubility of the determination solution is more than or equal to 30g and the boiling point is less than or equal to 150 ℃, so that the determination time is saved.
Sodium salt aqueous solution for multi-selection of the determination solution, such as sodium chloride, sodium sulfate, sodium nitrate and the like; aqueous solutions of potassium salts such as potassium chloride, potassium nitrate, potassium sulfate, etc.
The measurement solution was an aqueous sodium chloride solution. The boiling point of the sodium chloride aqueous solution is proper, the solubility is relatively constant, and pure sodium chloride crystals do not absorb moisture and are very stable.
The set concentration of the test solution is an unsaturated inorganic salt solution in the working environment. The solubility changes along with the temperature, and if the determination is carried out under the non-constant temperature condition, the unsaturated solution is selected, so that the supersaturation phenomenon caused by the temperature change can be avoided. Compared with saturated solution, the unsaturated solution has lower viscosity and is easy to be sucked by a sampling pump.
The rinse solution is ultrapure water, purified water and deionized water. Ultrapure water and the like do not contain impurities which affect the measurement precision, and are low in price and convenient to use.
A sample injection volume measuring method using the sample injection volume measuring device of the ion chromatograph of the invention prepares a measuring solution of inorganic salt solution with set concentration and a prepared flushing liquid, and the measuring steps are as follows:
switching a sample injection valve to ensure that a transfer pump and a receiving bottle for conveying flushing liquid are not communicated with the interface of the quantitative ring, disconnecting the flushing liquid passage, connecting a sampling pump and the measured solution with the interface of the quantitative ring, connecting the measured solution passage, or connecting the sampling pump and a waste liquid pipe for conveying the measured solution with the interface of the quantitative ring, connecting the measured solution passage, starting the sampling pump, and conveying the measured solution with a set quantity into the quantitative ring; then, the sampling pump is closed, the sample introduction valve is switched, the sampling pump and the measuring solution are not communicated with the interface of the quantitative ring, the passage of the measuring solution is disconnected, or the sampling pump and the waste liquid pipe for conveying the measuring solution are not communicated with the interface of the quantitative ring, the passage of the measuring solution is disconnected, the infusion pump and the receiving bottle for conveying the flushing liquid are communicated with the interface of the quantitative ring, the passage of the flushing liquid is communicated, the infusion pump is started, the infusion pump conveys the flushing liquid to flush the measuring solution in the quantitative ring, and the flushing liquid and the measuring solution enter the receiving bottle; when the measuring solution conveyed by the sampling pump at one time reaches the weight capable of being weighed by the weighing mechanism, evaporating the collected flushing liquid and the measuring solution to separate out crystal salt in the measuring solution, calculating the weight of the measuring solution conveyed into the quantitative ring according to the set salt concentration of the measuring solution, and calculating the accurate volume of the measuring solution conveyed into the quantitative ring by the set amount according to the density of the inorganic salt solution of the measuring solution at the temperature during measurement; when the measuring solution once delivered into the quantitative ring by the sampling pump is not enough for the weighing mechanism to weigh, repeating the switching of the sample injection valves, starting the sampling pump again, conveying a set amount of the determination solution into the quantitative ring, starting the infusion pump, conveying flushing fluid to flush the determination solution in the quantitative ring until the determination solution conveyed by the sampling pump for N times reaches or exceeds the weight capable of being weighed by the weighing mechanism, evaporating the collected flushing fluid and the determination solution, and separating out crystalline salt in the determination solution, calculating the weight of the measured solution which is conveyed into the quantitative ring for N times according to the set concentration of the measured solution, calculating the accurate volume of the determined solution with the set quantity conveyed into the quantitative ring for N times according to the density of the determined solution inorganic salt solution at the temperature during the determination, the exact volumes of the test solution delivered N times are simply arithmetically averaged to calculate the exact volume of the set amount of test solution delivered into the quantification loop for each time. The sample injection volume measuring method using the sample injection volume measuring device of the ion chromatograph has the advantages of reliable measured sample injection volume and high precision.
When the volume of the full ring of the quantitative ring is measured, the passage of the measuring solution is communicated, the sampling pump is started, and the set quantity of the measuring solution conveyed into the quantitative ring is 2-4 times of the volume of the full ring of the quantitative ring. The testing solution which is 2 to 4 times of the volume of the quantitative ring is conveyed to realize the internal rinsing of the pipeline, thereby greatly improving the pollution elimination level.
The invention has the advantages that: the invention relates to a sample injection volume measuring device of an ion chromatograph, which is used for accurately measuring the sample volume in a full quantitative loop sample injection mode and a partial quantitative loop sample injection mode. The determination solution adopts an inorganic salt solution with a set concentration, the washing liquid washes the determination solution in the quantitative ring, the washing is clean and has no residue, salt crystals in the determination solution have no loss, and the determination result is accurate; the sample injection volume measuring method using the sample injection volume measuring device of the ion chromatograph is reliable and has high measuring precision.
Drawings
FIG. 1 is a schematic structural diagram of an embodiment of an ion chromatograph sample injection volume measuring device according to the present invention;
fig. 2 is a schematic structural diagram of another embodiment of the ion chromatograph sample injection volume determination device of the invention.
Detailed Description
Fig. 1 and fig. 2 are schematic structural diagrams of two embodiments of the ion chromatograph sample injection volume determination device of the invention. The description is combined with the drawings.
Example one
The sample injection valve 2 of the embodiment shown in fig. 1 is a six-way valve, and 1-6 ports are sequentially arranged; the both ends of ration ring 1 are connected 1 interface and 4 interfaces respectively, and the entry linkage flush fluid 6 of transfer pump 7, 2 interfaces of exit linkage injection valve 2, and 3 interfaces of injection valve 2 are connected to receiving bottle 5, and 6 interfaces of injection valve 2 are connected to sampling pump 4, and 3 connections 5 interfaces of injection valve 2 are connected to survey solution. When the sample injection valve 2 is switched to the connection of the interfaces 2 and 3, the interfaces 1 and 6 are connected, and the interfaces 4 and 5 are connected, the infusion pump 7 and the receiving bottle 5 cannot be connected with the interface of the quantitative ring 1, the flushing liquid passage is disconnected, the sampling pump 4 and the measuring solution 3 are connected with the interface of the quantitative ring 1, and the measuring solution passage is connected; when the sample injection valve 2 is switched to the connection of the interfaces 1 and 2, the interfaces 3 and 4 are connected, and the interfaces 5 and 6 are connected, the sampling pump 4 and the measured solution 3 cannot be connected with the interface of the quantitative ring 1, the passage of the measured solution is disconnected, the infusion pump 7 and the receiving bottle 5 are connected with the interface of the quantitative ring 1, and the passage of the flushing liquid is connected. The sampling pump 4 is an injection pump controlled in an electric control calculation mode, and the stepping motor drives a piston rod to move so as to suck and discharge the measured solution 3. Fig. 1 shows a suction type sampling method in which a sampling pump 4 sucks a measurement solution 3 into a quantitative ring 1. The determination solution 3 is an inorganic salt solution with a set concentration, in this embodiment, 100 g of water and 30g of an unsaturated aqueous solution of sodium chloride are selected, and the unsaturated solution has lower viscosity compared with a saturated solution and is easy to be sucked by the sampling pump 4; the selected rinsing liquid 6 is required to be a non-toxic and harmless liquid which does not chemically react with the measurement solution 3, and the selected rinsing liquid 6 has no solid solute residue or extremely trace amount of residue in the process of evaporating the crystallized salt precipitated from the rinsing liquid 6 and the measurement solution 3, which does not affect the measurement accuracy, such as ultrapure water, purified water, deionized water and the like. The rinse solution 6 of this embodiment is purified water. The weighing mechanism of this embodiment is an analytical balance.
Example two
The difference between the embodiment shown in FIG. 2 and the embodiment shown in FIG. 1 is that the inlet of the sampling pump 4 is connected to the measurement solution 3, the outlet is connected to the port 6 of the sample injection valve 2, and the waste liquid pipe 8 is connected to the port 5 of the sample injection valve 2. This is an injection sampling method, wherein the measuring solution 3 is sucked into the sampling pump 4, and then injected into the quantitative ring 1, and the excess waste liquid is discharged through the waste liquid pipe 8.
EXAMPLE III
In this example, a sample volume measurement method using the measurement apparatus of the first example was used, and the measurement solution 3 was prepared by using an aqueous solution of 30g of sodium chloride with a set concentration of 100 g, and the washing solution 6 was purified water. The determination step comprises:
the injection valve 2 is switched so that the transfer pump 7 and the receiving bottle 5 are not connected to the interface of the quantitative ring 1, the flushing fluid passage is disconnected, the sampling pump 4 and the measurement solution 3 are connected to the interface of the quantitative ring 1, and the measurement solution passage is connected. The sampling pump 4, namely the injection pump, firstly carries out zero calibration on the movement of a piston rod of the injection pump before starting, then calculates the stroke of the piston rod of the injector by rotating a motor, controls the injection pump to convey 100.00 microliter of sodium chloride aqueous solution with a nominal value into the quantitative ring 1, and measures the current air temperature of 25 ℃; then, the sampling pump 4 is closed, the sample injection valve 2 is switched, the sampling pump 4 and the measured solution 3 are not communicated with the interface of the quantitative ring 1, the passage of the measured solution is disconnected, the infusion pump 7 and the receiving bottle 5 are communicated with the interface of the quantitative ring 1, the passage of the flushing solution is communicated, the infusion pump 7 is started, the infusion pump 7 delivers 250.00 microliters of purified water to flush the sodium chloride aqueous solution in the quantitative ring 1, and the purified water and the sodium chloride aqueous solution enter the receiving bottle 5; the sodium chloride water solution that sampling pump 4 once carried and got into quantitative ring 1 is not enough the weight that weighing mechanism analytical balance can weigh, repeats the aforesaid and switches injection valve 2, until when sampling pump 4 totally 8 times carry the sodium chloride water solution, 100.00 microlitres each time, totally 800.00 microlitres, can satisfy analytical balance and weigh, evaporate pure water and sodium chloride water solution, precipitate 0.2320 grams of crystalline salt in the sodium chloride water solution, pure sodium chloride crystallization is not hygroscopic, and is very stable. The weight of 1.020 g delivered into the quantitative ring 1 was calculated for 8 times based on the set concentration of the aqueous sodium chloride solution, the exact volume of the set amount of the measured solution 3 delivered into the quantitative ring 1 was calculated to be 791.4 microliters based on the density of the aqueous sodium chloride solution of the set concentration at the measurement temperature of 25 ℃ being 1.290 g/ml, the simple arithmetic mean of the exact volumes of the measured solutions 3 for 8 times was 98.93 microliters, and the measurement results showed that the error was 1.2% when the nominal value of the syringe pump was 100.00 microliters. In the same way, a plurality of nominal volume values of the syringe pump of the sampling pump 4 can be determined. In the determination, the evaporation degree of the purified water is similar to that of the sodium chloride aqueous solution, and the determination process is simple, convenient and quick. The sampling volume measuring method using the sampling volume measuring device of the ion chromatograph is reliable and has high precision.
Example four
The present embodiment is another sample volume measurement method using the measurement device of the first embodiment, and the difference between the present embodiment and the third embodiment is: controlling the injection pump to deliver a sodium chloride aqueous solution with a full-ring quantitative value of 900.20 microliters to the quantitative ring 1 at one time, switching the injection valve 2 when the sodium chloride aqueous solution delivered by the injection pump reaches the weight capable of being weighed by the analytical balance, delivering 2500.00 microliters of purified water by the infusion pump 7 to flush the sodium chloride aqueous solution in the quantitative ring 1, evaporating the collected purified water and the sodium chloride aqueous solution, and separating out the crystal salt in the sodium chloride aqueous solution0.300And g, calculating the weight of the sodium chloride aqueous solution conveyed into the quantitative ring 1 to be 1.147 g according to the set concentration of the sodium chloride aqueous solution, calculating the accurate volume of the full-ring sodium chloride aqueous solution conveyed into the quantitative ring 1 to be 889.4 microliter according to the density of the sodium chloride aqueous solution with the set concentration at the measurement temperature of 25 ℃ to be 1.290 g/ml, and determining the result to show that the error of the nominal value of the full ring injected into the quantitative ring by the injection pump is 1.2 percent.
EXAMPLE five
The present embodiment is a sample injection volume measurement method using the measurement device of the second embodiment, which is different from the fourth embodiment in that: switching the sample injection valve 2 to make the infusion pump 7 and the receiving bottle 5 not connected with the interface of the quantitative ring 1, disconnecting the flushing liquid passage, connecting the sampling pump 4 and the waste liquid pipe 8 for conveying the measured solution 3 with the interface of the quantitative ring 1, connecting the measured solution passage, controlling the injection pump to convey the sodium chloride aqueous solution to the quantitative ring 1, then closing the sampling pump 4, switching the sample injection valve 2, disconnecting the sampling pump 4 and the waste liquid pipe 8 for conveying the sodium chloride aqueous solution with the interface of the quantitative ring 1, and disconnecting the measured solution passage.
EXAMPLE six
The present embodiment is a sample injection volume measurement method using the measurement device of the second embodiment, which is different from the third embodiment in that: switching the sample injection valve 2 to make the infusion pump 7 and the receiving bottle 5 not connected with the interface of the quantitative ring 1, disconnecting the flushing liquid passage, connecting the sampling pump 4 and the waste liquid pipe 8 for conveying the measured solution 3 with the interface of the quantitative ring 1, connecting the measured solution passage, controlling the injection pump to convey the sodium chloride aqueous solution to the quantitative ring 1, then closing the sampling pump 4, switching the sample injection valve 2, disconnecting the sampling pump 4 and the waste liquid pipe 8 for conveying the sodium chloride aqueous solution with the interface of the quantitative ring 1, and disconnecting the measured solution passage.
Claims (7)
1. A kind of ion chromatograph advances the volume determination device, including two interfaces that the both ends of the quantitative ring (1) connect the sample valve (2) respectively; a sampling pump (4) conveys the determination solution (3) into the quantitative ring (1); the sampling pump (4) is communicated with the interface of the sampling valve (2), the quantitative ring (1) and the determination solution (3) is communicated with the interface of the sampling valve (2) to form a determination solution passage, or the sampling pump (4) is communicated with the interface of the sampling valve (2), the quantitative ring (1) and the waste liquid pipe (8) is communicated with the interface of the sampling valve (2) to form a determination solution passage; a receiving bottle (5) and a weighing mechanism, and is characterized in that an infusion pump (7) conveys flushing liquid (6) into the quantitative ring (1); the infusion pump (7) is communicated with the interface of the sample injection valve (2), the quantitative ring (1) and the receiving bottle (5) is communicated with the interface of the sample injection valve (2) to form a flushing fluid passage; switching the sample injection valve (2) to connect the quantitative ring (1) with the measuring solution passage or to connect the quantitative ring (1) with the washing solution passage; the measuring solution (3) is an inorganic salt solution with a set concentration, the washing liquid (6) does not react with the measuring solution (3), and the washing liquid (6) has no solid solute residue or extremely trace residue in the process of evaporating and precipitating inorganic salt from the washing liquid (6) and the measuring solution (3) and does not influence the measuring precision.
2. The ion chromatograph sampling volume measuring device of claim 1, wherein the sampling valve (2) is a six-way valve, and 1-6 interfaces of the six-way valve are sequentially arranged; the two ends of the quantitative ring (1) are respectively connected with the interface 1 and the interface 4, the infusion pump (7) connected with the flushing liquid (6) is connected with the interface 2 of the sample injection valve (2), the receiving bottle (5) is connected with the interface 3 of the sample injection valve (2), the sampling pump (4) is connected with the interface 6 of the sample injection valve (2), and the measuring solution (3) is connected with the interface 5 of the sample injection valve (2).
3. The ion chromatograph sampling volume measuring device of claim 1, wherein the sampling valve (2) is a six-way valve, and 1-6 interfaces of the six-way valve are sequentially arranged; the two ends of the quantitative ring (1) are respectively connected with the interface 1 and the interface 4, an infusion pump (7) connected with flushing liquid (6) is connected with the interface 2 of the sample injection valve (2), a receiving bottle (5) is connected with the interface 3 of the sample injection valve (2), a sampling pump (4) connected with the measuring solution (3) is connected with the interface 6 of the sample injection valve (2), and a waste liquid pipe (8) is connected with the interface 5 of the sample injection valve (2).
4. The ion chromatograph sample injection volume determination device according to claim 1, 2 or 3, characterized in that the determination solution (3) has a solubility of more than or equal to 30g and a boiling point of less than or equal to 150 ℃ at a working environment temperature of 20-30 ℃.
5. The ion chromatograph sample introduction volumetric determination device according to claim 1, 2 or 3, characterized in that the rinsing liquid (6) is ultrapure water, purified water and deionized water.
6. A sample volume measuring method using the sample volume measuring apparatus of any one of claims 1 to 5, characterized in that a measuring solution (3) of an inorganic salt solution of a set concentration is prepared, a rinsing solution (6) is prepared, and the measuring step:
switching a sample injection valve (2), so that a liquid conveying pump (7) for conveying flushing liquid (6) and a receiving bottle (5) are not communicated with the interface of the quantitative ring (1), the flushing liquid passage is disconnected, a sampling pump (4) and a measuring solution (3) are communicated with the interface of the quantitative ring (1), the measuring solution passage is communicated, or the sampling pump (4) for conveying the measuring solution (3) and a waste liquid pipe (8) are communicated with the interface of the quantitative ring (1), the measuring solution passage is communicated, starting the sampling pump (4), and conveying a set amount of measuring solution (3) into the quantitative ring (1); then, the sampling pump (4) is closed, the sample injection valve (2) is switched, the sampling pump (4) and the measuring solution (3) are not communicated with the interface of the quantitative ring (1), the passage of the measuring solution is disconnected, or the sampling pump (4) and the waste liquid pipe (8) which convey the measuring solution (3) are not communicated with the interface of the quantitative ring (1), the passage of the measuring solution is disconnected, the infusion pump (7) which convey the flushing liquid (6) and the receiving bottle (5) are communicated with the interface of the quantitative ring (1), the passage of the flushing liquid is connected, the infusion pump (7) is started, the infusion pump (7) conveys the flushing liquid (6) to flush the measuring solution (3) in the quantitative ring (1), and the flushing liquid (6) and the measuring solution (3) enter the receiving bottle (5; when the measuring solution (3) conveyed by the sampling pump (4) for one time reaches the weight capable of being weighed by the weighing mechanism, evaporating the collected flushing liquid (6) and the measuring solution (3) to separate out crystal salt in the measuring solution (3), calculating the weight of the measuring solution (3) conveyed into the quantitative ring (1) according to the set salt concentration of the measuring solution (3), and calculating the accurate volume of the set amount of the measuring solution (3) conveyed into the quantitative ring (1) according to the density of the inorganic salt solution of the measuring solution (3) at the temperature during measurement; when the sampling pump (4) once conveys the measuring solution (3) entering the quantitative ring (1) to be less than the weight capable of being weighed by the weighing mechanism, the switching of the sample injection valve (2) is repeated, the sampling pump (4) is restarted, the measuring solution (3) with set quantity is conveyed to enter the quantitative ring (1), the infusion pump (7) is started, the flushing liquid (6) is conveyed to flush the measuring solution (3) in the quantitative ring (1) until the measuring solution (3) conveyed by the sampling pump (4) for N times reaches or exceeds the weight capable of being weighed by the weighing mechanism, the collected flushing liquid (6) and the measuring solution (3) are evaporated to separate out the crystal salt in the measuring solution (3), the weight of the measuring solution (3) conveyed into the quantitative ring (1) for N times is calculated according to the set concentration of the measuring solution (3), the density of the inorganic salt solution (3) is measured according to the temperature at the measuring time, the accurate volume of the set amount of the measuring solution (3) which is conveyed into the quantitative ring (1) for N times is calculated, the simple arithmetic mean is calculated for the accurate volume of the measuring solution (3) which is conveyed into the quantitative ring (1) for N times, and the accurate volume of the set amount of the measuring solution (3) which is conveyed into the quantitative ring (1) each time is calculated.
7. The method of claim 6, wherein when the full loop volume of the quantification ring (1) is measured, the measurement solution passage is connected, the sampling pump (4) is started, and the set amount of the measurement solution (3) fed into the quantification ring (1) is 2 to 4 times the full loop volume of the quantification ring.
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| CN111426777B (en) * | 2020-06-12 | 2020-11-27 | 赛默飞世尔（上海）仪器有限公司 | Method for determining pipeline volume, liquid chromatography system and pipeline volume determining device |
| CN114636456B (en) * | 2022-05-18 | 2022-08-23 | 江苏省计量科学研究院(江苏省能源计量数据中心) | Quantitative ring volume calibration system and method |
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