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4.
4.
In an acidic medium, the sample solution is analyzed with an atomic absorption spectrophotometer with an air acetylene flame
4.
4.
4.
4.
4.
4.
4.
4.
4.
4.
Nickel 232.
4.
4.
Determination of iron and copper: Weigh 1g sample (accurate to 0.
001g), dissolve it in water, add 2ml hydrochloric acid solution, quantitatively transfer it to a 25mL volumetric flask, dilute to the mark with water, and shake well
.
Determine nickel: Weigh 1g sample (accurate to 0.
001g), dissolve it in water, add 2mL hydrochloric acid solution, transfer quantitatively to a 100mL volumetric flask, dilute to the mark with water, and shake well
.
4.
5.
4.
2 Drawing of standard curve
Take 1.
00mL, 2.
00mL, 4.
00mL, 8.
00mL of copper and iron standard solutions respectively, and take 2.
00mL, 4.
00mL, 6.
00mL, 8.
00mL of nickel standard solutions and place them in a 100ml volumetric flask respectively.
Dilute to the mark with water and shake well.
, Make a standard series of solutions
.
Set the operating conditions of the atomic absorption spectrophotometer according to the instrument manual, adjust the wavelength according to 4.
5.
3.
4, introduce the standard series of solutions into the atomic absorption spectrophotometer, adjust the zero with water, measure the absorbance, and draw a standard curve of absorbance versus concentration
.
4.
5.
4.
3 Determination of samples
The sample solution is introduced into the atomic absorption spectrophotometer, the absorbance is measured, and the concentration of the element is found from the standard curve
.
4.
5.
5 Expression of analysis results
The content (X i ) of an element expressed in mass percentage is calculated according to formula (3):
Where: V—volume of sample, mL;
c i —the concentration of an element in the sample, mg/L;
mi—the mass of the sample, g
.
4.
5.
6 Allowance
Take the arithmetic average of the two measurement results as the measurement result
.
The relative deviation of the two parallel determination results shall not be greater than 20%
.
4.
6 Determination of alkali metals and alkali metals
4.
6.
1 Method summary
Under ammonia conditions, all metal ions in the sample except alkali metal and alkaline earth metal ions form sulfide precipitates with hydrogen sulfide
.
Sulfuric acid is added to the filtrate to make the alkali metal and alkaline earth metal ions exist in the form of sulfate , and it is burned at a high temperature to a constant quality
.
4.
6.
2 Reagents and solutions 4.
6.
2.
1 Ammonia
.
4.
6.
2.
2 Sulfuric acid
.
4.
6.
2.
3 Hydrogen sulfide
.
4.
6.
3 Analysis steps
Weigh 1g sample (accurate to 0.
01g), place it in a 100mL graduated test tube, add 80mL water and 10mL ammonia to dissolve, add water to 100mL, and mix
.
Pass in hydrogen sulfide to saturate it, filter with dry filter paper, and discard about 20 mL of the initial filtrate
.
Take 50ml of the filtrate and place it in a porcelain crucible with constant quality, add 0.
2ml of sulfuric acid , evaporate it to dryness on a hot plate, and then burn at (800±25)℃ until the quality is constant
.
4.
6.
4 Expression of analysis results
The content (X 3 ) of alkali metals and alkaline earth metals expressed in mass percentage is calculated according to formula (4):
In the formula: m 1 -crucible mass, g;
m 2 ——the mass of crucible plus residue, g;
m—The mass of the sample.
g
.
4.
6.
5 Allowance
Take the arithmetic mean of the two parallel determination results as the determination result
.
The difference between the two parallel determination results shall not be greater than 0.
05%
.
5 Inspection rules
5.
1 This product should be inspected by the quality inspection department of the manufacturer
.
The manufacturer shall ensure that the products manufactured are in compliance with the requirements of this standard, and shall be accompanied by a quality certificate, which includes: the name of the manufacturer, site, product name, grade, batch number, net content, production date and serial number of this standard
.
5.
2 Taking products of the same quality as a batch, the volume of each batch shall not exceed 1000kg
.
5.
3 Determine the number of sampling units according to 6.
6 of GB/T6678-1986
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Sampling should meet the requirements of Chapter 2 in GB/T6679-1986
.
The sampling volume of each batch shall not be less than 500g
.
Mix the collected samples and put them into two clean and dry ground-mouth bottles
.
Label stating: manufacturer name, product name, batch number, sampling date
.
One bottle is used for inspection, and the other bottle is kept for three months for future reference
.
5.
4 The test result is judged according to the rounding value comparison method in GB/T1250
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If one of the indicators in the inspection results does not meet the requirements of this standard, samples should be taken from twice the amount of packaging for re-inspection
.
Even if only one index does not meet the requirements of this standard in the re-inspection result, the whole batch of products is unqualified
.
6 Marking, packaging, transportation and storage
6.
1 The packaging container should be painted with firm and obvious signs, indicating: manufacturer name, product name, product grade, batch number, trademark, production date, and net content
.
6.
2 Industrial manganese acetate is packed in plastic drums or cardboard drums lined with plastic bags, and the inner plastic bag needs to be tied
.
6.
3 During transportation, load and unload lightly, avoid collision, and prevent sunlight, rain and moisture
.
6.
4 Industrial manganese acetate should be stored in a cool and ventilated warehouse or shed
.
Related Links: Industrial Manganese Acetate (2)