CN114814070A - Method for measuring bromate content in drinking water - Google Patents
Method for measuring bromate content in drinking water Download PDFInfo
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- CN114814070A CN114814070A CN202210301224.0A CN202210301224A CN114814070A CN 114814070 A CN114814070 A CN 114814070A CN 202210301224 A CN202210301224 A CN 202210301224A CN 114814070 A CN114814070 A CN 114814070A
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- SXDBWCPKPHAZSM-UHFFFAOYSA-M bromate Inorganic materials [O-]Br(=O)=O SXDBWCPKPHAZSM-UHFFFAOYSA-M 0.000 title claims abstract description 75
- SXDBWCPKPHAZSM-UHFFFAOYSA-N bromic acid Chemical compound OBr(=O)=O SXDBWCPKPHAZSM-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 238000000034 method Methods 0.000 title claims abstract description 47
- 239000003651 drinking water Substances 0.000 title claims abstract description 42
- 235000020188 drinking water Nutrition 0.000 title claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 90
- 238000001514 detection method Methods 0.000 claims abstract description 46
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000002414 normal-phase solid-phase extraction Methods 0.000 claims abstract description 25
- 229910052709 silver Inorganic materials 0.000 claims abstract description 25
- 239000004332 silver Substances 0.000 claims abstract description 25
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 20
- 238000005342 ion exchange Methods 0.000 claims abstract description 12
- 238000004458 analytical method Methods 0.000 claims abstract description 8
- 238000002347 injection Methods 0.000 claims abstract description 4
- 239000007924 injection Substances 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 9
- 150000001450 anions Chemical class 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 239000012224 working solution Substances 0.000 claims description 3
- 239000003480 eluent Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 230000008929 regeneration Effects 0.000 claims description 2
- 238000011069 regeneration method Methods 0.000 claims description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 230000035945 sensitivity Effects 0.000 abstract description 6
- 239000000523 sample Substances 0.000 description 77
- 238000011084 recovery Methods 0.000 description 18
- 239000000460 chlorine Substances 0.000 description 11
- 238000010438 heat treatment Methods 0.000 description 11
- 229910052500 inorganic mineral Inorganic materials 0.000 description 7
- 239000011707 mineral Substances 0.000 description 7
- 235000010755 mineral Nutrition 0.000 description 7
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 6
- -1 chlorine ions Chemical class 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 238000004255 ion exchange chromatography Methods 0.000 description 4
- 238000004659 sterilization and disinfection Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000012086 standard solution Substances 0.000 description 3
- 235000020682 bottled natural mineral water Nutrition 0.000 description 2
- 230000035622 drinking Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 239000012468 concentrated sample Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000835 electrochemical detection Methods 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012421 spiking Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/96—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation using ion-exchange
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
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Abstract
The invention provides a method for measuring bromate content in drinking water, which comprises the following steps: s1, pretreatment of the water sample: concentrating the water sample, and then removing chloride ions in the concentrated water sample by using a silver solid-phase extraction column; s2, sample injection analysis: and filtering the water sample pretreated in the step S1, feeding the filtered water sample into an ion exchange chromatograph for detection, and substituting the detection result into a standard curve to determine the content of bromate. The invention establishes a detection method of the bromate in the drinking water, which has higher sensitivity and lower detection limit, and solves the problem of low accuracy of the detection result of the detection method of the bromate in the drinking water in the prior art.
Description
Technical Field
The invention belongs to the field of bromate content detection, and particularly relates to a method for determining the bromate content in drinking water.
Background
The ozone disinfection technology is an advanced and safe method in the current drinking water disinfection method, but researches show that the ozone can generate bromate with bromide in water in the disinfection process of the drinking water, the bromate is internationally recognized as a 2B-level potential carcinogen, and the limit value of the bromate is regulated to be 10 mu g/L by the world health organization's Drinking Water quality Standard' and the current 'domestic Drinking Water health Standard' in China.
At present, the measuring method of the bromate content in drinking water mainly comprises an ion chromatography method, a high performance liquid chromatography method and a capillary electrophoresis-electrochemical detection method. The ion chromatography is popularized and used due to the advantages of rapidness, simplicity, convenience, sensitivity, good selectivity, low detection cost and the like, and the bromate detection method in the current national standard GB8538-2016 natural mineral water for drinking of food safety is also used for measuring the content of bromate in drinking water by using the ion chromatography.
The quantitative limit of the bromate detection method in the GB8538-2016 national food safety standard natural mineral water drinking detection method in the current national standard is 5 mug/L, and the quantitative limit is closer to the limit of 10 mug/L of bromate in the current national standard drinking water, so that the problem of low accuracy of detection results in the determination of the content of bromate in the drinking water by using the standard exists, and the detection results do not meet the standard requirements. Therefore, the problem of low detection result accuracy of the drinking water bromate detection method in the existing standard can be solved by establishing the bromate detection method with higher sensitivity and lower detection limit.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide a method for measuring the content of bromate in drinking water, so as to establish a method for detecting the bromate in the drinking water, which has higher sensitivity and lower detection limit, and solve the problem that the detection result of the method for detecting the bromate in the drinking water in the prior art is low in accuracy.
The invention provides a method for measuring bromate content in drinking water, which comprises the following steps:
s1, pretreatment of the water sample: concentrating the water sample, and then removing chloride ions in the concentrated water sample by using a silver solid-phase extraction column;
s2, sample injection analysis: and filtering the water sample pretreated in the step S1, feeding the filtered water sample into an ion exchange chromatograph for detection, and substituting the detection result into a standard curve to determine the content of bromate.
General Cl in mineral water - The content is far higher than BrO 3- High concentration of Cl due to the relatively close time of the two - BrO is easily caused by overhigh concentration after concentration 3- Poor separation and even covering of BrO 3- In the case of peak shape, the detection recovery rate of bromate is low due to high content of chloride ions, and the accuracy of experimental determination is influenced, so that the influence of chloride ions in a sample needing to be removed is avoided, and a silver solid-phase extraction column is selected to remove the chloride ions with too high concentration. Aiming at removing chloride ions in a sample, the method firstly concentrates a water sample so as to obviously reduce the volume of the water sample to be detected, and then utilizes a silver solid-phase extraction column to treat the concentrated water sample, so that the chloride ions in the water sample can be effectively removed, the interference of a chloride ion chromatographic peak on a bromate chromatographic peak is eliminated, the detection limit of the bromate content detection of drinking water is reduced, and the sensitivity of the bromate content detection of the drinking water is improved. The drinking water bromate detection method provided by the scheme is utilized to control the quality index of the drinking water, so that the safety of the drinking water can be further improved. On the other hand, the water sample to be detected adopts a treatment method of firstly concentrating and then passing through the silver solid-phase extraction column, so that the column passing time of each sample can be shortened, the volume of the water sample to be detected can be controlled below the sample volume bearing threshold value of the silver solid-phase extraction column, and the silver solid-phase extraction column can ensure that the Cl in the water sample to be detected is treated by the silver solid-phase extraction column - Play effectual effect of getting rid of, be favorable to improving the chloride ion separation efficiency of silver solid phase extraction post, reduce the detection consumptive material cost and the operating time cost that the drinking water detected, have the value of popularization and application.
Preferably, in S2, the water sample is concentrated by a direct heating method. The common water sample concentration methods include a microwave heating method and a water bath heating method, but the microwave heating method is not suitable for long-time batch treatment of the water sample, and the water bath heating method consumes too long time and is easy to generate pollution. And utilize the concentrated water sample of direct heating method, it is short just can concentrate the processing water sample in batches for a long time consuming time, in addition add glass pearl in order to avoid bumping when the direct heating process, guaranteed the security of water sample heating concentration process.
Preferably, the water sample is concentrated by a factor of not less than 5.
Preferably, the water sample is concentrated by a factor of 5. The concentration multiple not less than 5 times can ensure that the recovery rate of the water sample is better and the recovery rate is not different, the concentration mode of 5 times is short in time consumption, and the problem that mineral substances are separated out from the water sample with the too high concentration multiple is avoided.
Preferably, the silver solid phase extraction column is a 1.00cc size silver siebol solid phase extraction column.
Preferably, the analysis system of the ion exchange chromatograph is an anion separation column and an anion protection column.
Preferably, the anion separation column is a Switzerland Metrosep A Supp-250 anion column, and the anion protection column is a Switzerland Metrosep A Supp 415Guard4.0 protection column.
Preferably, the eluent of the ion exchange chromatograph is a mixed solution of 3.0-3.5 mmol/L sodium carbonate and 0.8-1.2 mmol/L sodium bicarbonate.
Preferably, the regeneration liquid of the ion exchange chromatograph is 0.3-0.5 wt% of dilute sulfuric acid solution.
Preferably, the flow rate of the leacheate is 0.6-0.8 mL/min.
Preferably, the elution pattern of the eluate is isocratic.
Preferably, in the step S2, the volume of the water sample fed into the ion exchange chromatograph is 150-350 μ L. By adopting a larger sample injection amount, the content of bromate in detection is increased, so that the detection error can be reduced, and the detection limit of the bromate is reduced.
Preferably, in S2, the standard curve is Y ═ AX + B, where a ranges from 0.0003 to 0.0007, B ranges from 4E-06 to 7E-06, X is the bromate concentration, and the ordinate Y is the bromate peak area.
Preferably, the standard working solution concentration of the standard curve is 1. mu.g/L, 5. mu.g/L, 10. mu.g/L, 25. mu.g/L, 50. mu.g/L, 100. mu.g/L.
Preferably, the method meets the application condition, and the bromate content in the drinking water to be detected is 1-100 mug/L.
Compared with the prior art, the method has the advantages that the chlorine ions in the water sample are removed after the water sample is concentrated, on one hand, the detection limit and the quantitative limit of bromate in the water sample are reduced by concentrating the water sample, the sensitivity and the accuracy of bromate detection in the drinking water are improved, on the other hand, the chlorine ions in the water sample are removed after the water sample is concentrated, the volume of the water sample passing through the silver solid phase extraction column is ensured to be within the bearing threshold value of the silver solid phase extraction column, and the purpose of effectively removing the chlorine ions in the water sample is achieved. Through the mode that combines to get rid of chloride ion interference behind making the water sample concentrated, solved among the prior art that detection quantitation limit is too high and lead to the not high problem of testing result degree of accuracy.
Drawings
FIG. 1 is an ion chromatogram of different modes of eliminating chloride ions;
FIG. 2 shows 5-fold BrO concentration 3 - With Cl - A resolution map;
FIG. 3 shows 10-fold BrO concentration 3 - With Cl - A resolution map;
FIG. 4 shows BrO 3 - A standard curve.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.
The standard curve of the standard solution used for measuring the bromate content in the water samples of the following examples is 0.0005X +6E-06 (R0.9999), as shown in fig. 4, where X is the bromate concentration and Y is the bromate peak area on the ordinate. The standard working solution concentrations of the standard curve were 1. mu.g/L, 5. mu.g/L, 10. mu.g/L, 25. mu.g/L, 50. mu.g/L, 100. mu.g/L.
Example 1: influence of different modes for removing chloride ions on effect of removing chloride ions in water sample
The water sample is concentrated by a direct heating method in the embodiment, and the specific operations are as follows: taking a water sample in a clean beaker, and directly putting the beaker on an electric furnace to concentrate the water sample.
In order to select a suitable way for removing chloride ions, this embodiment performs ion chromatography on a water sample that passes through the silver solid-phase extraction column first and then is concentrated to enrich bromate ions, and a water sample that does not pass through the silver solid-phase extraction column concentrated respectively, where the water sample that does not pass through the silver solid-phase extraction column concentrated is a blank control group, and an experimental result is shown in fig. 1. As can be seen from the figure: the water sample to be detected is made to pass through the silver solid phase extraction column and then concentrated, and the silver solid phase extraction column removes Cl - Has a poor effect, and fails when the sample amount passing through the silver solid phase extraction column reaches a certain volume, in which case the silver solid phase extraction column is sensitive to Cl - The removal effect of (a) is not ideal; however, the water sample to be detected is concentrated and enriched firstly, and then the concentrated water sample passes through the silver solid phase extraction column, so that the chloride ion peak in the obtained water sample ion chromatogram is basically completely disappeared, which indicates that the operation can well remove the chloride ion in the water sample, and eliminates the interference of the chloride ion chromatogram peak on the bromate chromatogram peak.
Example 2: influence of different concentration times on water sample recovery rate
According to the experimental result in example 1, the pretreatment of the water sample in this example adopts a method of first concentrating the water sample and then removing chloride ions in the water sample through the silver solid phase extraction column. On the basis of directly heating the concentrated water sample, the embodiment determines the appropriate concentration factor by studying the relationship between the concentration factor of the concentrated water sample and the recovery rate of the bromate as the measured substance.
The specific operation of this embodiment is: taking 12 clean beakers, dividing into two groups, each group comprises 6 beakers, adding 50mL of water sample into one group, and adding 2.5mL of BrO into 3 water samples 3 - Standard solution (100. mu.g/L), the remaining 3 water samples as blanks, the water samples of this group were concentrated 5 times; the other group is added with 100mL of water samples respectively, and 3 water samples are added with 5.0mL of BrO 3 - Standard solution (100. mu.g/L), the remaining 3 water samples as blanks, the water sample set was concentrated 10 times; directly placing the beakers on an electric furnace to heat in groups, concentrating a water sample until the residual water sample in the beakers is less than 10mL, transferring a concentrated solution into a 10mL colorimetric tube, washing the beakers for 2-3 times by using ultrapure water, combining washing solutions into the 10mL colorimetric tube, fixing the volume to a 10mL scale mark, sequentially passing the solution with the fixed volume through a silver solid-phase extraction column and a filter membrane, measuring the solution with a computer, and substituting the obtained detection result into a standard curve to determine the content of bromate. As shown in table 1, fig. 2 and fig. 3, it is understood from table 1 that the average recovery rate of the water sample concentrated 5 times is 101.5%, and the average recovery rate of the water sample concentrated 10 times is 98.1%, and the difference between the average recovery rates is small. As can be seen from FIGS. 2 and 3, the BrO concentration of the same volume of water sample was 5 times and 10 times after the concentration 3 - With Cl - The separation degree is better, but when the concentrated sample with the same volume is concentrated, the time consumption for concentrating by 10 times is far longer than that for concentrating by 5 times, and the efficiency is relatively low; and for the sample with higher mineral content, after the sample is concentrated by 10 times, the mineral in the water sample is easy to separate out, the subsequent transfer and constant volume are influenced, the final detection result is further influenced, the factors are comprehensively considered, and the BrO enriched in the water sample by 5 times of concentration times is selected 3 - 。
TABLE 1 comparison of the results of the fold concentration measurements
Example 3: calculation of detection limit and quantitative limit and accuracy evaluation thereof
Based on the experimental results of example 2, the following pretreatment methods were applied to the water samples with low bromate content in this example: directly heating and concentrating for 5 times, and removing chloride ions in a water sample through a silver solid-phase extraction column.
And (3) feeding the pretreated water sample with low bromate content into an ion exchange chromatograph for analysis, and repeating the experiment for 7 times in parallel, wherein the test results are shown in table 2. And calculating the standard deviation S according to the actual concentration of bromate in the water sample to obtain the standard deviation S of 0.080. The detection limit MDL is calculated according to the following formula (1),
MDL＝t(6,0.99)·S (1)
wherein, t in the formula is 3.143, which is unilateral distribution with 6 degree of freedom and 99% confidence; s value 0.080, which is the standard deviation of 7 replicates. The detection limit of the detection method is calculated to be 0.25 mug/L, and the average concentration of the sample is 0.758 mug/L and is not more than 10 times of the detection limit of the calculated method, so that the concentration of the sample does not need to be measured again, and the detection limit has reasonableness. The 4-fold detection limit was used as the limit for this test, which was calculated to be 1.00. mu.g/L.
TABLE 2 data of 7 determinations of the same batch of water samples with low bromate content
In addition, in order to evaluate the accuracy of the detection method, the recovery rate and standard deviation of the detection method need to be analyzed and calculated. Selecting a water sample with the background content of 0.758 mug/L, and performing standard addition experiments according to 3 levels of 1-time quantitative limit (1.00 mug/L), 5-time quantitative limit (5.00 mug/L) and 10-time quantitative limit (national standard limit, 10.00 mug/L), wherein each level is subjected to parallel experiments for 6 times to calculate the recovery rate and the relative standard deviation, and the experiment results are shown in Table 3.
TABLE 3 BrO 3 - Recovery and relative deviation (n ═ 6)
From Table 3, BrO 3 - When the adding quantity of the standard deviation is 1 time of the quantitative limit, the recovery rate is 96.6-106.0 percent, the relative standard deviation is 3.2 percent, when the adding quantity of the standard deviation is 5 times of the quantitative limit, the recovery rate is 97.1-105.1 percent, the relative standard deviation is 3.1 percent, when the adding quantity of the standard deviation is 10 times of the quantitative limit, the recovery rate is 97.9-102.6 percent, and the relative standard deviation is 1.9 percent. From this, BrO 3 - When the additive amount of the bromate content in the drinking water is 1, 5 and 10 times, the recovery rate and the relative standard deviation are better, so that the method for measuring the bromate content in the drinking water has higher accuracy.
Example 4: verification of practical application of method
Based on the pretreatment and analysis steps of the water sample in example 3, the present example was verified in practical application of the method with the drinking water sold in the market as a verification index of recovery rate. The background content of bromate in 5 commercially available mineral waters of different product types was measured according to established methods, and 3 sets of parallel spiking tests were conducted on each of the 5 products, wherein the concentration of bromate in the spiked solution was 25. mu.g/L, and the results are shown in Table 4. The data in the table 4 show that bromate is detected in all 5 products, the bromate content meets the national standard requirement, and the average recovery rate is 93.2-98.0%, so that the method established by the invention has better accuracy, and the method can also well meet the requirement for measuring the bromate content in mineral water.
TABLE 45 recovery rates of commercial mineral waters
Example 5: determination of bromate content in enterprise samples
In order to sterilize drinking water with ozone, under the same processing conditions, the higher the concentration of ozone used for sterilization, the higher the concentration of bromate correspondingly generated, and this example performs bromate content determination on 4 batches of enterprise samples under the same processing conditions, wherein all the 4 batches of enterprise samples are sterilized with ozone, and the relevant sample parameters and bromate content determination results are shown in table 5. As can be seen from Table 5, the higher the concentration of ozone used in the process, the higher the bromate content in the final product, and the bromate content in the above 4 batches of enterprise samples was less than the international and national bromate limit of 10. mu.g/L, which meets the international and national standards.
TABLE 5 Enterprise sample analysis results
Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the true spirit and scope of the present invention.
Claims (10)
1. A method for measuring the bromate content in drinking water is characterized by comprising the following steps:
s1, pretreatment of the water sample: concentrating the water sample, and then removing chloride ions in the concentrated water sample by using a silver solid-phase extraction column;
s2, sample injection analysis: and filtering the water sample pretreated in the step S1, feeding the filtered water sample into an ion exchange chromatograph for detection, and substituting the detection result into a standard curve to determine the content of bromate.
2. The method for measuring the bromate content in drinking water according to claim 1, wherein: the concentration multiple of the water sample is not less than 5 times.
3. The method for measuring the bromate content in drinking water according to claim 1, wherein: the analysis system of the ion exchange chromatograph comprises an anion separation column and an anion protection column.
4. The method for measuring the bromate content in drinking water according to claim 3, wherein: the eluent of the ion exchange chromatograph is a mixed solution of 3.0-3.5 mmol/L sodium carbonate and 0.8-1.2 mmol/L sodium bicarbonate.
5. The method for measuring the bromate content in drinking water according to claim 4, wherein: the regeneration liquid of the ion exchange chromatograph is 0.3-0.5 wt% of dilute sulfuric acid solution.
6. The method for measuring the bromate content in drinking water according to claim 4, wherein: the flow rate of the leacheate is 0.6-0.8 mL/min.
7. The method for measuring the bromate content in drinking water according to claim 1, wherein: and in the S2, the volume of a water sample fed into the ion exchange chromatograph is 150-350 mu L.
8. The method for measuring the bromate content in drinking water according to claim 1, wherein: in the step S2, the standard curve is Y ═ AX + B, where a ranges from 0.0003 to 0.0007, B ranges from 4E-06 to 7E-06, X is bromate concentration, and Y on the ordinate is bromate peak area.
9. The method for measuring the bromate content in drinking water according to claim 8, wherein: the standard working solution concentration of the standard curve is 1 mug/L, 5 mug/L, 10 mug/L, 25 mug/L, 50 mug/L and 100 mug/L.
10. The method for measuring the bromate content in drinking water according to claim 1, wherein: the method meets the application condition, and the bromate content in the drinking water to be detected is 1-100 mu g/L.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0783890A (en) * | 1993-07-20 | 1995-03-31 | Yamazaki Baking Co Ltd | Determination method for bromate in bread using gas chromatograph mass spectrometer |
| CN103018184A (en) * | 2012-11-23 | 2013-04-03 | 上海理工大学 | Method for measuring trace amount of bromate in water |
| CN104090039A (en) * | 2014-07-08 | 2014-10-08 | 青海大学 | Method for simultaneously determining inorganic anions and organic acid radical ions in salt lake brine |
| US20180149627A1 (en) * | 2016-11-29 | 2018-05-31 | Sichuan University | Low pressure anion exchange chromatography-turbidimetric method for simultaneous online analysis of trace sulfide and chloride in water samples |
| CN108226371A (en) * | 2018-01-23 | 2018-06-29 | 杭州润泽科学器材有限公司 | A kind of method of trace bromate in measure bottled water |
| CN108956815A (en) * | 2018-07-05 | 2018-12-07 | 科之杰新材料集团有限公司 | The test method of chloride ion content in a kind of sea sand |
| CN112285245A (en) * | 2020-11-17 | 2021-01-29 | 湖南农业大学 | Gas chromatography-mass spectrometry method for detecting content of fluazinam in paddy field water body |
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Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0783890A (en) * | 1993-07-20 | 1995-03-31 | Yamazaki Baking Co Ltd | Determination method for bromate in bread using gas chromatograph mass spectrometer |
| CN103018184A (en) * | 2012-11-23 | 2013-04-03 | 上海理工大学 | Method for measuring trace amount of bromate in water |
| CN104090039A (en) * | 2014-07-08 | 2014-10-08 | 青海大学 | Method for simultaneously determining inorganic anions and organic acid radical ions in salt lake brine |
| US20180149627A1 (en) * | 2016-11-29 | 2018-05-31 | Sichuan University | Low pressure anion exchange chromatography-turbidimetric method for simultaneous online analysis of trace sulfide and chloride in water samples |
| CN108226371A (en) * | 2018-01-23 | 2018-06-29 | 杭州润泽科学器材有限公司 | A kind of method of trace bromate in measure bottled water |
| CN108956815A (en) * | 2018-07-05 | 2018-12-07 | 科之杰新材料集团有限公司 | The test method of chloride ion content in a kind of sea sand |
| CN112285245A (en) * | 2020-11-17 | 2021-01-29 | 湖南农业大学 | Gas chromatography-mass spectrometry method for detecting content of fluazinam in paddy field water body |
Non-Patent Citations (1)
| Title |
|---|
| 李婷婷 等: "离子色谱法同时测定饮用水中的溴酸盐和高氯酸盐", 食品工业, vol. 41, no. 9, pages 325 - 328 * |
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