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Flame hydride generator specification
Foreword
After years of research on flow injection of hydrides, it has been found in actual tests that the use of flames for hydride elements has the following advantages.
1 . Easy to use, the favorable conditions of the flame can be used as the basis, and the effective detection of As, pb. Se, Sb, Bi, Pb, Sn, Te, Ge can be performed without changing the condition .
2 . Fast , easy to use , and easy to operate.
3. Easy to clean , no memory effect. Â Â
Work on the development of analytical methods
1. Prepare a standard solution with a concentration of about 50-100 times sensitivity (0.2-0.5 Abs is optimal) and a blank solution to check or determine:
Chemical conditions that occur b. Conditions of the generator c. Conditions of the host d. Stability of the reading e. Actually achieved sensitivity (calculated by subtracting the blank reading).
2. Prepare a series of standard solutions, taking arsenic as an example: with 0, 0.1, 0.2, 0.4, 0.8, ug/ml, draw a standard curve. The range of standard solution solutions: up to about 100-150 times the sensitivity, must have a blank solution.
3. Preparation of potassium borohydride. Potassium borohydride KBH 4 (or sodium), most of the hydride elements used 1.5%. 1.5 g of potassium borohydride and 0.3 g of sodium hydroxide (stabilizer) were weighed into a plastic bottle (not available in a glass vessel), and dissolved in 100 ml of distilled water. One week at room temperature. 0.1% sodium hydroxide.
4. Pretreatment of the sample:
Dissolve the sample according to the relevant method. b. Whether a pre-reduction of the measured element is required. c. Dilute to a certain multiple so that the reading does not exceed the maximum measurable concentration (corrected after actual measurement) and meet the requirements of chemical conditions.
5. Check for the presence of interfering elements in the sample:
Observe the interference elements and interference quantities of the measured elements from the literature, and compare with the known coexisting elements of the test samples to determine whether it is necessary to control the interference. b. Check the presence or absence of interference with the recovery test: take 2 sample solutions, one plus a known amount of the measured element, one without adding, measure the content and then subtract, calculate the recovery. The recovery rate is considered to be interference-free at 100 ± 2%. When 100±5%, if there is a higher requirement, it is considered to have interference and needs to be controlled.
6. Interference control
Controlled by the methods provided in the literature and verified by recycling experiments. b. For unclear interference, or interference that cannot be completely eliminated, and the recovery rate of different addition amounts are similar, that is, there is “multiplication interferenceâ€, multiplying a coefficient to get the correct value, and “standard addition method†can be used. Determination. When there is "additional interference", it cannot be eliminated by the standard addition method.
7. Determine the standard sample and verify the correctness of the method used. Â Â Â Â Â Â Â Â Â Â Â Â Â Â Â Â Â Â
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II . Analysis methods of each element
Arsenic As
1. Wavelength: 193.7nm.
2. Arsenic (V valence) should be reduced to arsenic (III valence): add potassium iodide to the concentration of 0.5-1% (V/V) before adding to the sample or standard solution to be determined, and add ascorbic acid to a concentration of 0.2- After 0.5% constant volume, it is heated in a boiling water bath and the temperature is raised to about 80-90 ° C). After cooling, it can be measured.
3. Acidity of sample and standard solution: Constant volume with 10% hydrochloric acid (V/V,), the acidity in the literature is 1-9M.
4 linear range 0.1-10ug/mL (also in the range of 0.1-20ng/mL)
5 Sensitivity: Factory default 0.18 ug/mL/1% A. (Optimized to 0.08 ug/ml1%A), this sensitivity is measured with high-performance lamps and is related to the performance of the atomic absorption host. The sensitivity of the host is also different, and all subsequent sensitivity indicators are the same.
Selenium Se
1. Wavelength: 196.0 nm.
2. Selenium (VI price) is reduced to selenium (IV price): If the selenium in the standard solution is tetravalent, it may not be pre-reduced, and the hexavalent should be reduced. After the sample or standard is dissolved, add a few milliliters of hydrochloric acid (1:1), and use a common glass device to boil the solution. With polyethylene or polytetrafluoroethylene (PTFE) open-mouth flask, there was no loss when boiling.
Allow to cool off after heating for a few minutes.
3. Acidity: 20% (V/V) hydrochloric acid medium for sample and standard solution. The literature has an acidity of 2.5-5M.
4. Linear range 1-8ug/mL
5. Sensitivity: 0.32ug/mL/1%.
Lead Pb
1. Wavelength: 217.0 nm for high performance lamps and 283.3 nm for normal lamps.
2. Carrier gas flow: 150 ml/min.
3. Acidity: 0.5% (V/V) hydrochloric acid medium is used for both the sample and the standard solution. The literature has an acidity of 0.1-0.2M.
4. Oxidizer: Lead ion is usually 2 valence, lead in hydride is 4 valence, and oxidant should be added to the solution.
a. Use potassium ferricyanide oxidant (only for samples with low heavy metal content such as biological materials), the highest sensitivity. Add before constant volume, and make up to volume after dissolution. The concentration was 0.4% (0.8-1.0% in the literature).
b. The use of hydrogen peroxide, ammonium persulfate, potassium dichromate and other oxidants in the literature is less sensitive than potassium ferricyanide, but less interfering elements (see literature).
5. Linear range 1-20ug/mL
6. Sensitivity: 0.18ug/mL/1%. (Optimized by using potassium ferrocyanide oxidizer to reach 0.08ug/mL/1%).
Tin Sn
1 Wavelength: 286.3nm for ordinary lamps and 224.6 nm for high-performance lamps.
2. Carrier gas flow rate: 300 mL/min.
3. Acidity: 0.5% HCl (V/V) Document acidity 0.1-0.2M.
4. Linear range 10-80ug/mL
5. Sensitivity: 0.42ug/mL/1%A.
é“‹ Bi
1. Wavelength: 223.0 nm.
2. Carrier gas flow rate: 100 mL/min.
3. Acidity: 20% (V/V) hydrochloric acid. Literature acidity 1-9M
4. Linear range 10-80ug/mL
5. Sensitivity: 0.42ug/mL/1%A.
碲 Te
1. Wavelength: 214.3 nm.
2. Carrier gas flow rate: 150ml/min.
3. Reduce 碲(VI) to 碲(IV): Add concentrated hydrochloric acid to the sample or standard solution and boil for 1 minute (no loss).
4. Acidity: 20% (V/V) hydrochloric acid medium. Literature acidity 2.5-3
5. Linear range 10-80ug/mL
6. Sensitivity: 0.4ug/ml/1%A.
锑 Sb
1. Wavelength: 217.6nm.
2. 锑(V) is reduced to 锑(III), and 锑(V) is about 2 times less sensitive than 锑(III). The reduction method is the same as arsenic, but it can be completed instantaneously at normal temperature without heating.
3. Acidity: 10% hydrochloric acid (V/V). The literature has an acidity of 1-9M.
4. Linear range 5-70ug/mL
5. Sensitivity: 0.3ug/ml/1%A.
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