Hg3.0 Cold Atomic Absorption Mercury Analyzer User Manual
1 Overview
1.1 Purpose: Determination of trace mercury in all samples. Mercury content determination in drinking water, natural water, wastewater, soil, food and feed, biological samples, minerals, petroleum and its processed products can be completed according to current testing methods and standards.
1.2 Working principle: Atomic absorption spectroscopy measurement using long path technology.
1.3 Technical indicators
1.3.1 * Operating temperature: Room temperature to 40 ℃
1.3.2 * Environmental pressure: 84.0-106.7 kPa
1.3.3 Working power supply: 220VAC, 50Hz, power 5W.
1.3.4 * * Scope: The testing range for mercury content in the solution is 0.5-100 μ g/L.
Linear error (%)<5, * * limit (ng/mL)<0.5, 15ng/L repeatability<3%
1.5ng/L repeatability<3%, optical path: mercury vapor optical path 200mm, controlled by Windows interface.
2 List
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serial number
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name
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quantity
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serial number
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name
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quantity
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1
|
host
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1 unit
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8
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10 μ L syringe
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1 unit
|
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2
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220V50Hz power cord
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1 piece
|
9
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50 μ L syringe
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1 unit
|
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3
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USB line
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1 piece
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10
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100 μ L syringe
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1 unit
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4
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Flipping bottle rack
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1 piece
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11
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2.5 μ g/mL mercury standard solution
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5mL (2 units)
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5
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5mL foam bottle
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2 of them
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12
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40% stannous chloride
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50mL (1 bottle)
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6
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5mL freezer tube
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5
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13
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Instruction Manual
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1 book
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|
7
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Standard reagent rack
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1 piece
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|
|
|
3 Installation
3.1 Whole machine installation
3.2 Software Installation
Copy the Hg3 folder to the D drive, double-click on the file in the Hg3 folder
Icon installation software. In the Hg3 folder
Send icon to desktop.
3.3 Startup: Double click the Hg3 icon to enter the interface shown in Figure 3.3. Click to enter the next interface.
Figure 3.3 Homepage
4 Reagent preparation
All water used in the analysis process is deionized water, and the chemical reagents used are analytical grade or superior grade.
4.1 Nitric acid (high-purity).
4.2 Sulfuric acid (high-purity)
4.3 Hydrochloric acid (high-purity).
4.4 Nitric acid potassium dichromate solution (5+0.05+94.5): Weigh 0.5g of potassium dichromate and place it in water. Add 50mL of nitric acid and dilute with 1000mL of water.
4.5 Stannous chloride solution (40%): Weigh 200g of stannous chloride and add it to a 500mL beaker. Add 500mL of 6mol/L hydrochloric acid and heat it in a boiling water bath to make it colorless and transparent.
4.6 Mercury standard solution
4.6.1 Mercury standard stock solution: Weigh about 0.2g of pure mercury using an analytical balance, add it to a 1000mL volumetric flask, record the accurate value (0.0001g), add 10mL of nitric acid (high-purity) water, dissolve it in boiling water, dilute it with nitric acid potassium dichromate solution to the mark, and mix well. Label concentration.
4.6.2 2.50 μ g/mL mercury standard solution (solution A): Take the mercury standard reserve solution (containing 1.2500mg mercury) and add it to a 500mL volumetric flask to make up to volume. This solution contains 2.500 μ g of mercury per mL.
4.6.3 0.250 μ g/mL mercury standard solution (solution B): Diluted 10 times from solution A. This solution contains 0.250 μ g of mercury per mL.
4.6.4 Digestive agent: 200ml nitric acid+50ml sulfuric acid+50ml 0.5% ammonium metavanadate.
All glassware used must be soaked overnight in nitric acid (1+5), rinsed repeatedly with water, and rinsed thoroughly with deionized water. The digestive tract is 200mm in length and 40mm in outer diameter.
5 Interface * Creation
5.1 Click "Enter" to enter the main interface of the Hg3.0 mercury analyzer.
5.2 Writing File Names
5.3 Setting the Range, Quantitative Basis, and Measurement Time in Sampling Conditions
5.4 Setting Experimental Parameters
6 Measurement standard solution
6.1 Instrument conditions: Turn on the mercury analyzer and preheat for 10 minutes. Gas flow rate is 0.5L/min.
6.2 Increase or decrease the number of standard series
6.3 Writing standard concentration values
Draw the standard curve by taking 2.00mL of stannous chloride solution (40%) and adding it to a boiling flask. Add 5.00mL of water and
Check the baseline button to check for ventilation foam * no mercury peak absorption. Click on the standard series table
On the second line, click
Add a 10 μ L syringe into a 10.0 μ L * Erlenmeyer flask of solution A and measure the absorption peak A1.
Click on the third row of the standard series table, then click
Button. Add a 100 μ L syringe into a 20.0 μ L * Erlenmeyer flask of solution A and measure the absorption peak A2.
Click on the fourth row of the standard series table and click the button. Add a 100 μ L syringe into a 30.0 μ L * Erlenmeyer flask of solution A and measure the absorption peak A3.
Click on the fifth row of the standard series table and click the button. Add a 100 μ L syringe into a 40.0 μ L * Erlenmeyer flask of solution A and measure the absorption peak A4.
Click on the sixth row of the standard series table and click the button. Add a 100 μ L syringe into a 60.0 μ L * Erlenmeyer flask of solution A and measure the absorption peak A5.
7 Sample Measurement
7.1 Sample processing takes dairy measurement as an example. Move the digestion instrument into a ventilated kitchen and preheat it to 160 ℃. Weigh 0.500g of dairy product and 3 glass beads into a digestive tube, then add 5.0ml of mixed acidPlace the digestive tube into the digestion apparatus, digest at 130 ℃ without any brown gas, add 5mL of water and heat for 10 minutes. Remove and cool, with a constant volume of 25mL marked on the scale. Extract 5.00mL for measurement, sample qualityQuantity=0.1g. Under the same conditions, prepare * * solution without adding sample.
7.2 Write sample measurement parameters: Write sample quantity=4, sample name=dairy product, sample size m=0.1, constant volume Vx=5. click
7.3 Measurement * * Wo
The fourth row has a sample name of * *, a sample size of m=1, and a constant volume of Vx=5,
Write 0 in the text box. Suck 2.00mL of stannous chloride solution (40%) and add it to a boiling bottle. Let it breathe and pour until there is no mercury peakAbsorption. Click on the fourth row of the X sample content calculation table,
Click the button. Use a 5ml pipette to aspirate 5.00mL of the digested * * solution, add it to a * boiling flask, and measure the sample absorption peak Ao=0.0061Refer to Figure 7.3. Click the "Calculate" button, and the calculation result is shown in Figure 7.3. At
Write * * Wo=3.26, Figure 7.4.
7.4 Determination of sample content
Take 2.00mL of stannous chloride solution (40%) and add it to a boiling bottle. Breathe and pour the bottle until there is no mercury peak absorption. Click on the first row of the X sample content calculation table, and then click
Button. Use a 5ml pipette to aspirate 5.00mL of digested solution (excluding oil and sediment), add it to a boiling flask, and measure the absorption peak Ax of the sample. Measure other samples in sequence, as shown in Figure 7.4.
7.5 Calculate sample size
Click the calculation button, and the calculation result is shown in Figure 7.4.
Sample size X (μ g/Kg)=(CxVx Wo)/m
Where:
Parabolic regression equation: Cx=a+ba+ccA
Cx - mercury concentration in the sample solution, μg/L;
A - absorbance measured by the sample;
a. B, c - parabolic coefficient
Sample size X=(CxVx Wo)/m
Vx - constant volume, mL
Wo --- * * The mass of mercury in * *, ng
M - sample quality, g
Expression of results: Report the two significant figures of the arithmetic mean.