This standard specifies the determination method of fluoride, chloride, bromide ions, nitrate and sulfate in natural drinking mineral water. This standard is applicable to the determination of fluoride, chloride, bromide ions, nitrate and sulfate in natural drinking mineral water. The detection limits of this method are: F-0.01 mg/L, Br 0.01 mg/L, CI-0.01 mg/L, NO3 0.025 mg/L, SO,2-0.025 mg/L, GB/T 5009.167-2003 Determination of fluoride, chloride, bromide ions, nitrate and sulfate in natural drinking mineral water by reverse phase high performance liquid chromatography GB/T5009.167-2003 Standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
GB/15009.167—2003
Determination of F-,Cl-,Br-.NO,-,SO,2- ionsin drinking water from natural mineral springbyreversedHPLC
2003-07-11Promulgated
Ministry of Health of the People's Republic of China
Standardization Administration of China
2004-01-01Implementation
GR/T5009.167-—2003
This standard is issued and imported by the Ministry of Health of the People's Republic of China, and the drafting unit of this standard is Chongqing Municipal Bureau of Industrial Biosafety. Drafters of this standard: Qi Guohua and Chen Yueming 386
1 Scope
Determination of fluoride, chlorine, nitrate and nitrate content in drinking natural mineral water by reversed phase high performance filtration chromatographywww.bzxz.net
GB/T 5009.167—2003
This standard specifies the method for the determination of fluoride, chlorine, bromine and nitrate content in natural mineral water. This standard is applicable to the determination of fluoride, chlorine, nitrate and nitrate content in natural mineral water. The maximum limits of this method are: F-0.7mg/:., B-001mg/1,1-0,0-mg, NFC.025mg/LS-.25mg/. 2 Principle
Under normal circumstances, since the anions do not produce color closure, they cannot be detected by external detection. However, when the mobile phase contains acid, for example, it can produce a high background. When a sample without anions flows through the detector, the decrease in absorption leads to a negative signal, which can be reversed by a rapid change in the recorded data. In this detection system, the retention time of anions in the sample is fixed. This characteristic of the sample anions can be used for qualitative analysis, and at the same time the mass concentration of the anions in the sample is correlated with the negative electrons. The height of the mark (or the area of ​​the bee), is proportional to the height of the mark. This relationship can be used to perform quantitative analysis. 3 Reagents || tt || 3.1 Preparation of mobile phase Take 81CmL of mobile phase and place it in a 10mL reagent bottle with a barrier film that has been cleaned before. There is a magnet in the bottle. Connect the reagent bottle to the vacuum pump with a hose, and place the bottle on the electric batch machine. Start it, open the pump, and absorb for 1 second to remove carbon dioxide in the system. Stop the system, add 100mL of phthalic acid into the reagent bottle, cover the bottle and then pump for 15 seconds. After stopping, add 140mL of ethyl acetate into the reagent bottle and suction with vacuum recorder for 15min: stop again, then add 2.1mL mol/1.0 sodium hydroxide solution into the reagent bottle, start stirring and use a pre-filtered single-seat meter to measure the pH of the trial solution. The pH of the solution is about 6-7: then add 1.1n0l/mol of sodium hydrogen sulfide dropwise to adjust the pH of the solution in the reagent bottle to 8.6±3.2. Factory standard reserve concentration of chemical (1.21 mg/mL): weigh 2.2100g of the solution that has been refracted in a medium at a rate of 1.2 mL in a small amount of pure water and transfer it into a new volume.
3.3 Oxidation standard preparation micron 1.9mg/m Weigh 1.4% 1* sodium chloride in 500~6ml pure water, transfer to 1001ml volumetric flask to make up to volume. 3.4 Miscellaneous standard leakage circulation equipment is (1.03)mg/m1.7, take 1. 1R CB is dried in a dryer. The potassium carbonate is added to a small amount of pure water and transferred to 10 liters or bottles.
3.5 Standard preparation solution of sodium sulfate (3.000m%/ml.): Take 1.5310K and dry it at 120~13C for 7 days. Then transfer it to 1 liter bottle in pure water to make up the volume.
3.6 Standard preparation solution of sulfate 1.0g/-TJ: Weigh 1.141K potassium carbonate that has been dried at 115℃ for 21 hours and add it to a small amount of pure water. Add 1C95m. and make up the volume in a bottle.
3.7 Sodium hydroxide concentration: 1.0m.ol/L.0.1mol /L3.8 According to the standard, the liquid must be used to absorb the fluoride, fluoride, bromide, and sulfate at room temperature, respectively, and the standard reserve of 3.2, 3.3, 3.4, 3.5, 3.6, 10. (L5). 00.5. ml.. n, nmi.5 n, mt. J1n00m in a volumetric bottle, and the water content is determined. The concentrations of nitrogen, chloride, iodide, sodium ion, and sulfur ion in this liquid are 13.0 mg/L, 50.0 mg/L, 5.0 mg/L, 50.0 mg/L, and 50.0 mg/L respectively: 4
GB/T 5009. 167—2003
4 Equipment
4.1 Commercial efficiency is only, the area is in (the period is ten residence), external detector 4.2 Speed ​​makes · s5 heart
4.3 The number of traps is really concentrated, CM0.15 type.
4.4 Membrane filter: water, c.45urm, 4.5 Ultrapure water, LFW-10N type.
5 Point discount ticket
5.1 Water sample is present
The clear water sample is directly passed through 0.45m water film and then , the mixed water needs to be filtered and then passed through a 0.4 μm water membrane for determination: 5.2 Determination
5.21 Suspected conditions
Temperature: 407:
Range of motion phase again! rLmin
Natural length 265nt
Sample, ).,25 (motor injection.
5.2.2 Qualitative analysis
Inject 25 μL of the sample and record the color increase. According to the normal time, the types of ions are determined in descending order: F-, HrNU, ,so-
5.2.3 Adjustment analysis
Determine the corresponding quotient (peak surface area) of each ion and quantify it by standard curve method. 5.2.4 Preparation of standard curve
5.2.4.1 Pipette 2.00ml5.00m10.um, 20.01ul50.00ml of the standard curve respectively and dilute to volume with pure water in 6 1-meter-high flasks. The quality of each ion in the prepared standard series is shown in Table 1. ·Customer
Reduction degree/(ang/1.>
5.2.4.2 Take the ignition flux as the model coordinate and the peak height (or peak return) as the pseudo coordinate to respectively construct the standard curves of F-, C-, Br-, NO\, S0,
6 auxiliary results calculation
Then the following formula is:
… The flux of water and the single energy dissociation of grams per liter A-, 3:, NO, and 8O- are obtained from the sample on the standard freezing curve. The unit step is grams per liter
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