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National food safety standard Determination of calcium, iron, zinc, sodium, potassium, magnesium, copper and manganese in foods for infants and young children, milk and milk products
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GB 5009.268-2016
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Detail Information of GB 5009.268-2016; GB5009.268-2016
Description (Translated English): National food safety standard Determination of calcium, iron, zinc, sodium, potassium, magnesium, copper and manganese in foods for infants and young children, milk and milk products
Sector / Industry: National Standard
Classification of Chinese Standard: C53; X82
Classification of International Standard: 67.100.10
Word Count Estimation: 16,167
Date of Issue: 2016-12-23
Date of Implementation: 2017-06-23
Older Standard (superseded by this standard): GB 5413.21-2010 Partial; GB/T 23545-2009; GB/T 23374-2009; GB/T 18932.11-2002; SN/T 0856-2011 Partial; SN/T 2208-2008; SN/T 2056-2008; SN/T 2049-2008; SN/T 2207-2008; NY/T 1653-2008
Regulation (derived from): National Health and Family Planning Commission Notice No.17 of 2016
Issuing agency(ies): National Health and Family Planning Commission of the People Republic of China, State Administration of Food and Drug Administration
Summary: This standard specifies inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma emission spectroscopy (ICP-OES) for multi-element determination in food. The first method applies to foods such as boron, sodium, magnesium, potassium, calcium, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc, arsenic, selenium, strontium, molybdenum, cadmium, tin , Barium, mercury, thallium, and lead. The second method is applicable to the determination of aluminum, boron, barium, calcium, copper, iron, potassium, magnesium, manganese, sodium, nickel, phosphorus, strontium, titanium, Determination.
GB 5009.268-2016
National food safety standard Determination of calcium, iron, zinc, sodium, potassium, magnesium, copper and manganese in foods for infants and young children, milk and milk products
National Standards of People's Republic of China
National Food Safety Standard
Multi-element determination in food
Issued on: 2016-12-23
2017-06-23 implementation
National Health and Family Planning Commission People's Republic of China
China Food and Drug Administration released
Foreword
This standard replaces GB 5413.21-2010 "national food safety standard infant foods and dairy products, calcium, iron, zinc, sodium, potassium, magnesium, copper
And manganese determination "in the second method, GB/T 23545-2009" Liquor manganese by inductively coupled plasma atomic emission spectrometry "
GB/T 23374-2009 "food in aluminum by inductively coupled plasma mass spectrometry", GB/T 18932.11-2002 "honey potassium,
Determination of inductively coupled plasma atomic phosphorus, iron, calcium, zinc, aluminum, sodium, magnesium, boron, manganese, copper, barium, titanium, vanadium, nickel, cobalt, chromium emission
Spectroscopy (ICP-AES) method ", SN/T 0856-2011" Detection of tin in canned food import and export, "the second law, SN/T 2208-
2008 "in aquatic products by microwave sodium, magnesium, aluminum, calcium, chromium, iron, nickel, copper, zinc, arsenic, strontium, molybdenum, cadmium, lead, mercury, selenium digestion - inductively coupled plasma
Plasma - mass spectrometry ", SN/T 2056-2008" Tea Import and Export of lead, arsenic, cadmium, copper, iron content was measured by inductively coupled plasma raw
Emission spectrometry ", SN/T 2049-2008" import and export food-grade phosphoric acid copper, nickel, lead, manganese, cadmium, titanium by inductively coupled plasma
Atomic emission spectrometry ", SN/T 2207-2008" Determination of the import and export of food additives DL- tartaric inductance of arsenic, cadmium, lead content
Coupled plasma atomic emission spectrometry ", NY/T 1653-2008" Vegetables, fruits and products measured by inductively coupled Mineral Elements
Plasma - Atomic Emission Spectrometry. "
This standard compared with GB 5413.21-2010 second method, the main changes are as follows:
--- Standard name was changed to "national food safety standards of food in multi-element determination";
--- Increased by inductively coupled plasma mass spectrometry as a first method;
--- Modification by inductively coupled plasma atomic emission spectrometry as the second method;
--- Modify the scope of application;
--- Modify the contents of the sample preparation section;
--- Modify the sample digestion in part;
--- Increasing the limit of detection and limit of quantification.
National Food Safety Standard
Multi-element determination in food
1 Scope
This standard specifies the multi-element determination in foods by inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma atomic emission
Spectroscopy (ICP-OES).
The first method is suitable for use in food boron, sodium, magnesium, aluminum, potassium, calcium, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc, arsenic, selenium, strontium, molybdenum, cadmium, tin, antimony ,
Barium, mercury, thallium, lead measurement; second method is suitable for use in food aluminum, boron, barium, calcium, copper, iron, potassium, magnesium, manganese, sodium, nickel, phosphorus, strontium, titanium, vanadium, zinc
Determination.
The first Inductively Coupled Plasma Mass Spectrometry (ICP-MS)
Principle 2
After digestion samples, as determined by inductively coupled plasma mass spectrometry, elemental specific mass number (mass to charge ratio, m/z) qualitative, external standard
Law to analyte mass signal intensity and the internal standard element mass ratio of the signal is proportional to the concentration of analyte quantitative analysis.
3 Reagents and materials
Unless otherwise indicated, the reagents used in this method are excellent pure water as a water GB/T 6682 regulations.
3.1 Reagents
3.1.1 nitric acid (HNO3): excellent pure or higher purity.
3.1.2 argon (Ar): argon (≥99.995%) or liquid argon.
3.1.3 helium (He): helium (≥99.995%).
3.1.4 elemental gold (Au) solution (1000mg/L).
3.2 reagent preparation
3.2.1 nitric acid solution (595): Take 50mL of nitric acid was slowly added 950mL of water, and mix.
3.2.2 Mercury standard stabilizer: Take 2mL element gold (Au) solution, diluted with nitric acid solution (595) to 1000mL, for mercury standard solution
The prepared liquid.
NOTE: Mercury standard stabilizer can also use 2g/L-cysteine hydrochloride nitrate (595) mixed solution, or other equivalent stabilizers.
3.3 Standard
3.3.1 element stock solution (1000mg/L or 100mg/L): lead, cadmium, arsenic, mercury, selenium, chromium, tin, copper, iron, manganese, zinc, nickel, aluminum, antimony, potassium,
Sodium, calcium, magnesium, boron, barium, strontium, molybdenum, thallium, titanium, vanadium and cobalt, and adopted by the National Certification Standards certificates granted single element or elements of the standard reservoir
Preparation of liquid.
3.3.2 internal standard stock solution (1000mg/L): scandium, germanium, indium, rhodium, rhenium, bismuth and other uses by the National Certification Standards and awarded certificates
Single element or elements of internal standard stock solution.
3.4 Standard Solution
3.4.1 mixed standard working solution: draw an appropriate amount of the stock standard solution or single-element multi-element mixed standard stock solution (595) by using a nitric acid solution
Stage dilution series dubbed mixed standard working solution, the concentration of each element in Table A.1.
NOTE: According to the sample digestion solution elements in quality levels, appropriate adjustments to each element concentration range of the standard series.
3.4.2 mercury standard solution: take the right amount of mercury stock solution with the mercury standard stabilizer stepwise dilution series dubbed in standard working solution concentration range
Table A.1.
3.4.3 internal standard solution: take the appropriate amount of internal standard stock solution or a single element within the standard multi-element standard stock solution to prepare a suitable solution of nitric acid (595)
Concentration of internal standard solution, an internal standard concentration see A.2.
Note: The standard solution either manually dosed in the preparation of mixed standard working solution and samples digest, can join online by the instrument.
4 instruments and equipment
4.1 Inductively coupled plasma mass spectrometry (ICP-MS).
4.2 Balance: a sense of 0.1mg and 1mg.
4.3 Microwave Digestion: digestion with Teflon inner tank.
4.4 pressure digestion tank: the inner tank with a Teflon digestion.
4.5 Ovens.
4.6 temperature control heating plate.
4.7 ultrasonic water bath.
4.8 Sample crushing equipment: homogenizer, high-speed grinder.
Step 5 Analysis
5.1 Sample Preparation
5.1.1 solid samples
5.1.1.1 dry sample
Beans, grains, mushrooms, tea, dried fruits, baked goods and other low water samples taken edible part, by the high-speed mill flour if necessary
Crushed uniform; for solid dairy products, protein powder, flour and other powdered sample showed a uniform shape, shake.
5.1.1.2 FRESH
Vegetables, while fruit, aquatic products, high moisture content of the sample is necessary washed, dried, take the edible part uniformly homogenized; for meat, eggs and other samples
Take edible part homogenized uniform.
5.1.1.3 frozen and canned foods
After thawing frozen foods and canned samples, whichever is the edible part of the homogenized uniform.
5.1.2 Liquid Sample
Soft drinks, spices and other samples shake.
5.1.3 Semi-solid samples
Stir well.
5.2 Sample Digestion
Note: You can select the appropriate method of digestion and digestion vessel based on the levels and the level of detection of analyte in the sample requirements.
5.2.1 Microwave Digestion
Weigh the solid sample 0.2g ~ 0.5g (accurate to 0.001g, more water samples containing the sample volume can be increased to 1g) or accurate shift
Take 1.00mL ~ 3.00mL liquid sample in microwave digestion within the tank, the sample containing ethanol or carbon dioxide to low heat on a hot plate
The ethanol was removed or carbon dioxide, nitric acid was added 5mL ~ 10mL, stamped or overnight place 1h, tighten the lid, in accordance with standard microwave digestion
Procedure digestion (digestion reference conditions Table B.1). After cooling out, slowly open the lid exhaust, rinsed with a small amount of water cover,
Digestion tank temperature on a hot plate or ultrasonic water bath heated 30min or ultrasonic degassing 2min ~ 5min at 100 ℃, water volume
To 25mL or 50mL, mixing spare, while doing the blank test.
5.2.2 pressure tank Digestion
Weigh the solid dry sample 0.2g ~ 1g (accurate to 0.001g, more water samples containing the sample volume can be increased to 2g) or accurate pipetting
Liquid sample 1.00mL ~ 5.00mL in digestion within the tank, the sample containing ethanol or carbon dioxide to a hot plate heated to remove low B
Alcohol or carbon dioxide, nitric acid was added 5mL placed 1h or overnight, tighten stainless steel jacket, put in oven temperature digestion (digestion reference conditions
Table B.1), at 150 ℃ ~ 170 ℃ digestion 4h, cooled, slowly loosen the stainless steel jacket, inside the digestion tank taken out in a temperature controlled hot plate
Or ultrasonic water bath heated at 100 ℃ 30min or ultrasonic degassing 2min ~ 5min, water volume to 25mL or 50mL, mix
Alternate, while doing the blank test.
5.3 Instrument Reference conditions
5.3.1 Instrument Operating Conditions: Instrument operating conditions, see Table B.2; Elemental Analysis mode Table B.3.
Note: there is no suitable instrument to eliminate the interference pattern, the interference correction equations requires the use of the measurement result correction, lead, cadmium, arsenic, molybdenum, selenium, vanadium and other elements of interference
Correcting equation shown in Table B.4.
5.3.2 Determination of reference conditions: After tuning the instrument to achieve the measurement requirements, measurement method editor, select the appropriate according to the nature of the analyte within the
m standard elements, measured elements and internal standard element/z Table B.5.
5.4 standard curve
The mixed standard solution is injected into inductively coupled plasma mass spectrometer to measure the value of the test signal response elements and internal standard element to be tested
Concentration of the element of the abscissa, the ratio of measured elements within the selected standard elements in response to the signal value of the vertical axis, the standard curve.
5.5 Determination of the sample solution
The blank solution and the sample solution were injected into the inductively coupled plasma mass spectrometer to measure the analyte and the internal standard element signal response
Value should give a concentration of the analyte in the digestion solution in accordance with the standard curve.
6 expression analysis
6.1 Calculation of the low levels of analyte
Content of the sample analyte low content according to formula (1):
X =
(Ρ-ρ0) × V × f
m × 1000
(1)
Where:
X --- the analyte content in the sample, in units of milligrams per kilogram or milligrams per liter (mg/kg or mg/L);
p --- sample solution tested element concentration in micrograms per liter (μg/L);
ρ0 --- blank sample solution tested element concentration, in micrograms per liter (μg/L);
V --- volume sample digestion volume in milliliters (mL);
f --- sample dilution;
m --- sample weighed mass or pipetting volume in grams or milliliters (g or mL);
1000 --- conversion factor.
The results to three significant figures.
6.2 Calculation of high levels of analyte
Content of the sample analyte by a high content of formula (2):
X =
(Ρ-ρ0) × V × f
(2)
Where:
X --- the analyte content in the sample, in units of milligrams per kilogram or milligrams per liter (mg/kg or mg/L);
ρ --- sample solution tested element concentration in milligrams per liter (mg/L);
ρ0 --- blank sample solution tested element concentration in milligrams per liter (mg/L);
V --- volume sample digestion volume in milliliters (mL);
f --- sample dilution;
m --- sample weighed mass or pipetting volume in grams or milliliters (g or mL).
The results to three significant figures.
7 precision
When samples of each element content greater than 1mg/kg, two independent determination results obtained under the repeatability condition must not exceed the absolute difference
Over 10% of the arithmetic mean; less than or equal to 1mg/kg and greater than 0.1mg/kg, twice under repeated conditions of independent testing
Given absolute difference may not exceed 15% of the arithmetic mean; less than or equal to 0.1mg/kg, under the same condition of two
Second independent determination of the absolute difference between the results should not exceed 20% of the arithmetic mean.
8 Other
Solid 0.5g sample volume to 50mL volume, liquid sample volume to 50mL 2mL volume calculation, the method of elements
The detection and quantitation limits in Table 1.
Table 1 inductively coupled plasma mass spectrometry (ICP-MS) detection limit and the limit of quantification
No. Element name The element symbol
The detection limit of 1
mg/kg
The detection limit of 2
mg/L
Limit of quantification 1
mg/kg
The limit of quantitation 2
mg/L
1 boron B 0.1 0.03 0.3 0.1
2 Na Na 1 0.3 3 1
3 Mg Mg 1 0.3 3 1
4 aluminum Al 0.5 0.2 2 0.5
5 K K 1 0.3 3 1
6 Calcium Ca 1 0.3 3 1
Table 1 (continued)
No. Element name The element symbol
The detection limit of 1
mg/kg
The detection limit of 2
mg/L
Limit of quantification 1
mg/kg
The limit of quantitation 2
mg/L
7 Titanium Ti 0.02 0.005 0.05 0.02
8 vanadium V 0.002 0.0005 0.005 0.002
9 chromium Cr 0.05 0.02 0.2 0.05
10 Mn Mn 0.1 0.03 0.3 0.1
11 Iron Fe 1 0.3 3 1
12 Cobalt Co 0.001 0.0003 0.003 0.001
13 Ni Ni 0.2 0.05 0.5 0.2
14 copper Cu 0.05 0.02 0.2 0.05
15 Zinc Zn 0.5 0.2 2 0.5
16 Arsenic As 0.002 0.0005 0.005 0.002
17 Selenium Se 0.01 0.003 0.03 0.01
18 Strontium Sr 0.2 0.05 0.5 0.2
19 Mo Mo 0.01 0.003 0.03 0.01
20 Cadmium Cd 0.002 0.0005 0.005 0.002
21 tin Sn 0.01 0.003 0.03 0.01
22 Antimony Sb 0.01 0.003 0.03 0.01
23 Ba Ba 0.02 0.05 0.5 0.02
24 Mercury Hg 0.001 0.0003 0.003 0.001
25 thallium Tl 0.0001 0.00003 0.0003 0.0001
26 Lead Pb 0.02 0.005 0.05 0.02
The second method by inductively coupled plasma atomic emission spectrometry (ICP-OES)
Principle 9
After sample digestion by inductively coupled plasma emission spectrometer, a characteristic element of wavelengths qualitative; analyte line letter
Proportional to the number and intensity of element concentrations were quantitatively analyzed.
10 Reagents and materials
Unless otherwise indicated, the reagents used in this method are excellent pure water as a water GB/T 6682 regulations.
10.1 Reagents
10.1.1 nitric acid (HNO3): excellent pure or higher purity.
10.1.2 perchloric acid (HClO4): excellent pure or higher purity.
10.1.3 argon (Ar): argon (≥99.995%) or liquid argon.
10.2 reagent preparation
10.2.1 nitric acid solution (595): Take 50mL of nitric acid was slowly added 950mL of water, and mix.
10.2.2 nitric acid - perchloric acid (101): Take 10mL of perchloric acid, nitric acid was slowly added to 100mL, and mix.
10.3 Standards
10.3.1 element stock solution (1000mg/L or 10000mg/L): potassium, sodium, calcium, magnesium, iron, manganese, nickel, copper, zinc, phosphorus, boron, barium, aluminum, strontium,
Vanadium and titanium, the use of certified and awarded by the National Standards certificate single element or multi-element standard stock solution.
10.3.2 Standard Preparation: Accurately draw an appropriate amount of a single element standard stock solution or multi-element mixed standard stock solution (595) by using a nitric acid solution
Stage dilution series dubbed mixed standard solution, the concentration of each element in Table A.2.
NOTE: According to the sample solution element concentration levels may be appropriate to adjust the standard series of the elements concentration range.
11 instruments and equipment
11.1 inductively coupled plasma emission spectrometer.
11.2 balance: a sense of 0.1mg and 1mg.
11.3 microwave digestion: digestion with Teflon inner tank.
11.4 pressure digester: equipped with a teflon digestion tank inside.
11.5 oven thermostat.
11.6 Adjustable temperature control heating plate.
11.7 muffle furnace.
11.8 Adjustable temperature electric furnaces.
11.9 Sample grinding apparatus: homogenizer, high-speed grinder.
12 analysis steps
12.1 Sample Preparation
With 5.1.
12.2 sample digestion
Note: You can select the appropriate method of digestion and digestion vessel based on the levels and the level of detection of the target element in the sample requirements.
12.2.1 Microwave Digestion
With 5.2.1.
12.2.2 pressure tank Digestion
With 5.2.2.
12.2.3 Wet Digestion
Accurately weigh 0.5g ~ 5g (accurate to 0.001g) or accurate Pipette 2.00mL ~ 10.0mL sample in a glass or Teflon consumption
Solution vessel, a sample containing carbon dioxide or ethanol to remove the ethanol and carbon dioxide over low heat on a hot plate, add 10mL of nitric acid - perchlorate
Acid (101) mixed solution to a hot plate or graphite digestion apparatus digestion, the digestion process if the digestion solution becomes dark brown, may be less suitable additional
The amount of acid mixture until white smoke, digestion colorless transparent or slightly yellow, cooling, water volume to 25mL or 50mL, mixing spare;
While doing the blank test.
12.2.4 Dry Digestion
Weigh accurately 1g ~ 5g (accurate to 0.01g) or accurate Pipette 10.0mL ~ 15.0mL sample into a crucible and placed 500 ℃ ~
550 ℃ in muffle furnace ashing 5h ~ 8h, cooled. If the ash is not completely black carbon particles, after cooling the solution of nitric acid a little wet in the electricity
After drying on a hot plate, muffle furnace continues to move into the ash white ash, cooling removed, dissolved in nitric acid solution was added 10mL and water volume
To 25mL or 50mL, mix standby; while doing the blank test.
12.3 Instrument Reference conditions
Optimization of instrument operation conditions, so that the sensitivity of the measured elements and other indicators have reached the requirements analysis, measurement method editor, select each test element together
Suitable analytical lines reference instrument operating conditions see B.3.1, analyte recommended analytical lines in Table B.6.
12.4 standard curve
The series of standard working solution into the inductively coupled plasma emission spectrometer to measure the intensity of the signal sounded analyte spectrum analysis
Should value, analyte concentration as the horizontal, its analytical line intensity value in response to the vertical axis, the standard curve.
12.5 Determination of the sample solution
The blank solution and the sample solution were injected into the inductively coupled plasma emission spectroscopy, the measurement of line intensities measured elemental analysis
Signal response, according to the standard curve to obtain the concentration of the analyte in the digestion solution.
13 analysis results presentation
Analyte content of the sample according to equation (3) Calculated:
X =
(Ρ-ρ0) × V × f
(3)
Where:
X --- the analyte content in the sample, in units of milligrams per kilogram or milligrams per liter (mg/kg or mg/L);
ρ --- sample solution tested element concentration in milligrams per liter (mg/L);
ρ0 --- blank sample solution tested element concentration in milligrams per liter (mg/L);
V --- volume sample digestion volume in milliliters (mL);
f --- sample dilution;
m --- sample weighed mass or pipetting volume in grams or milliliters (g or mL).
The results to three significant figures.
14 Precision
With Chapter 7.
Other 15
Solid 0.5g sample volume to 50mL volume, liquid sample volume to 50mL 2mL volume calculation, the method of elements
The detection and quantitation limits in Table 2.
Table 2 inductively coupled plasma atomic emission spectrometry (ICP-OES) detection limit and the limit of quantification
No. Element name The element symbol
The detection limit of 1
mg/kg
The detection limit of 2
mg/L
Limit of quantification 1
mg/kg
The limit of quantitation 2
mg/L
1 Al Al 0.5 0.2 2 0.5
2 Boron B 0.2 0.05 0.5 0.2
3 Ba Ba 0.1 0.03 0.3 0.1
4 Ca Ca 5 2 20 5
5 copper Cu 0.2 0.05 0.5 0.2
6 iron Fe 1 0.3 3 1
7 K K 7 3 30 7
8 Mg Mg 5 2 20 5
9 Mn Mn 0.1 0.03 0.3 0.1
10 Na Na 3 1 10 3
11 Ni Ni 0.5 0.2 2 0.5
12 P P 1 0.3 3 1
13 Strontium Sr 0.2 0.05 0.5 0.2
14 Titanium Ti 0.2 0.05 0.5 0.2
15 Vanadium V 0.2 0.05 0.5 0.2
16 Zinc Zn 0.5 0.2 2 0.5
Note: The sample preparation method and pressure microwave digestion tank Digestion.
Appendix A
The concentration of the standard solution series
A.1 ICP-MS method, the concentration of standard solution series Table A.1.
Table series standard solution concentration A.1 ICP-MS method elements
Reference element unit
Standard series concentration
Series 1 Series 2 Series 3 Series 4 Series 5 Series 6
1 B μg/L 0 10.0 50.0 100 300 500
2 Na mg/L 0 0.400 2.00 4.00 12.0 20.0
3 Mg mg/L 0 0.400 2.00 4.00 12.0 20.0
4 Al mg/L 0 0.100 0.500 1.00 3.00 5.00
5 K mg/L 0 0.400 2.00 4.00 12.0 20.0
6 Ca mg/L 0 0.400 2.00 4.00 12.0 20.0
7 Ti μg/L 0 10.0 50.0 100 300 500
8 V μg/L 0 1.00 5.00 10.0 30.0 50.0
9 Cr μg/L 0 1.00 5.00 10.0 30.0 50.0
10 Mn μg/L 0 10.0 50.0 100 300 500
11 Fe mg/L 0 0.100 0.500 1.00 3.00 5.00
12 Co μg/L 0 1.00 5.00 10.0 30.0 50.0
13 Ni μg/L 0 1.00 5.00 10.0 30.0 50.0
14 Cu μg/L 0 10.0 50.0 100 300 500
15 Zn μg/L 0 10.0 50.0 100 300 500
16 As μg/L 0 1.00 5.00 10.0 30.0 50.0
17 Se μg/L 0 1.00 5.00 10.0 30.0 50.0
18 Sr μg/L 0 20.0 100 200 600 1000
19 Mo μg/L 0 0.100 0.500 1.00 3.00 5.00
20 Cd μg/L 0 1.00 5.00 10.0 30.0 50.0
21 Sn μg/L 0 0.100 0.500 1.00 3.00 5.00
22 Sb μg/L 0 0.100 0.500 1.00 3.00 5.00
23 Ba μg/L 0 10.0 50.0 100 300 500
24 Hg μg/L 0 0.100 0.500 1.00 1.50 2.00
25 Tl μg/L 0 1.00 5.00 10.0 30.0 50.0
26 Pb μg/L 0 1.00 5.00 10.0 30.0 50.0
A.2 ICP-MS method using internal standard reference solution concentration.
Since the inner diameter of the peristaltic pump tubing used different instruments differently, when added to the standard line, so that should be considered within the standard element concentration in the sample liquid
Degrees, internal standard element reference concentration range of the sample solution after mixing was 25μg/L ~ 100μg/L, low-mass elements may be an appropriate increase in the use of liquid
concentration.
A.3 ICP-OES method series standard solution concentration shown in Table A.2.
Table series standard solution concentration A.2 ICP-OES method elements
Reference element unit
Standard series concentration
Series 1 Series 2 Series 3 Series 4 Series 5 Series 6
1 Al mg/L 0 0.500 2.00 5.00 8.00 10.00
2 B mg/L 0 0.0500 0.200 0.500 0.800 1.00
3 Ba mg/L 0 0.0500 0.200 0.500 0.800 1.00
4 Ca mg/L 0 5.00 20.0 50.0 80.0 100
5 Cu mg/L 0 0.0250 0.100 0.250 0.400 0.500
6 Fe mg/L 0 0.250 1.00 2.50 4.00 5.00
7 K mg/L 0 5.00 20.0 50.0 80.0 100
8 Mg mg/L 0 5.00 20.0 50.0 80.0 100
9 Mn mg/L 0 0.0250 0.100 0.250 0.400 0.500
10 Na mg/L 0 5.00 20.0 50.0 80.0 100
11 Ni mg/L 0 0.250 1.00 2.50 4.00 5.00
12 P mg/L 0 5.00 20.0 50.0 80.0 100
13 Sr mg/L 0 0.0500 0.200 0.500 0.800 1.00
14 Ti mg/L 0 0.0500 0.200 0.500 0.800 1.00
15 V mg/L 0 0.0250 0.100 0.250 0.400 0.500
16 Zn mg/L 0 0.250 1.00 2.50 4.00 5.00
Appendix B
Instrument reference conditions
B.1 digestion operation reference conditions
Digestion System Operation Reference conditions Reference Table B.1.
Table B.1 reference sample digestion conditions
Dispel step
temperature control
Heating time
min
Holding time
Microwave Digestion
1 120 5 5min
2 150 5 10min
3 190 5 20min
Pressure tank digestion
1 80 - 2h
2 120 - 2h
3 160 ~ 170 - 4h
B.2 inductively coupled plasma mass spectrometry (ICP-MS)
B.2.1 reference instrument operating conditions are shown in Table B.2.
Table B.2 inductively coupled plasma mass spectrometer operating conditions refer
Parameter name Parameters Name
RF power 1500W nebulizer high salt/Concentric Nebulizer
Plasma gas flow 15L/min sampling cone/skimmer nickel/platinum cone
The carrier gas flow rate 0.80L/min sampling depth 8mm ~ 10mm
Auxiliary gas flow 0.40L/min acquisition mode hopping peak (Spectrum)
Helium flow rate 4mL/min ~ 5mL/min Automatic Detection
Spray chamber temperature 2 ℃ per peak measurement points 1-3
Sample uptake rate 0.3r/s repetitions 2-3
B.2.2 Elemental analysis mode Reference Table B.3.
Table B.3 inductively coupled plasma mass spectrometry Elemental analysis mode
No. Element name The element analysis mode No. Symbol Name element symbol element analysis mode
1 ordinary boron B/collision cell 5 Normal potassium K/collision cell
2 Na Na General/collision cell 6 collision cell calcium Ca
3 collision cell magnesium Mg 7 Ti Ti collision cell
4 Al ordinary aluminum/vanadium V 8 collision cell collision cell
Table B.3 (Continued)
No. Element name The element analysis mode No. Symbol Name element symbol element analysis mode
9 chromium Cr collision cell 18 ordinary strontium Sr/collision cell
10 Mn Mn collision cell 19 Mo Mo collision cell
11 Iron Fe collision cell 20 Cd Cd collision cell
12 Cobalt Co collision cell 21 tin Sn collision cell
13 Ni Ni collision cell 22 Antimony Sb collision cell
14 Copper Cu collision cell 23 ordinary barium Ba/collision cell
15 Zinc Zn collision cell 24 ordinary mercury Hg/collision cell
16 As arsenic collision cell 25 ordinary thallium Tl/collision cell
17 Selenium Se collision cell 26 ordinary lead Pb/collision cell
B.2.3 element interference correction equations refer to Table B.4.
Table B.4 element interfer......
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