GB/T 631-2026Chemical reagent - Ammonia solution (English PDF)

1.0 L/min, Atomizing gas

0.7 L/min. Solution extraction rate.

1.2 mL/min. Analysis time. rinsing for 30 seconds, exposure for 5 seconds. The above instrument conditions can be optimized according to specific circumstances.

6.10.2.3 Determination Method Depending on the content of the analyte element in the sample, weigh 10g to 50g of the sample and place it in a quartz dish. Heat in a water bath or on an adjustable temperature electric plate. Evaporate and concentrate to approximately 5 mL on a hot plate. After cooling, transfer to a 25 mL volumetric flask, dilute to the mark with 5% nitric acid solution, and mix well. The determination shall be made in accordance with the provisions of

7.3.2 in GB/T 23942-2009, and the results shall be calculated in accordance with the provisions of

7.3.4 in GB/T 23942-2009.

6.3 Evaporation Residue Take 55 mL (50

g) of sample [110 mL (100

g) for high purity] and determine it according to GB/T 9740.

6.4.1.1 Preparation of test solution Take 110 mL (100

g) of sample, add

1.7 mL of sodium carbonate solution (50 g/L), evaporate to dryness in a water bath, dissolve the residue in water, and dilute. Up to 50 mL.

6.4.1.2 Determination Method Take 10 mL of the test solution, dilute it to 20 mL, and determine the turbidity according to GB/T 9729.The turbidity of the solution should not exceed the standard. Turbidity-sensitive solution. The standard turbidity solution is prepared by taking a standard solution containing

0.01 mg (analytical grade, superior grade) or

0.02 mg (chemically pure) chloride (Cl) solution. The solution was diluted to 20 mL and treated simultaneously with the same volume of the test solution.

6.4.2 Ion Chromatography

6.4.2.1 Reagents, Materials and Instruments Comply with the provisions of Chapters 5 and 6 of GB/T 34672-2017.

6.4.2.2 Instrument Conditions Chromatographic column. 250 mm length, 4 mm inner diameter; ethylstyrene-divinylbenzene polymer, alkanolic quaternary ammonium ion exchanger, particle size... It has a 9µm column and a pH tolerance range of 0-

14.Alternatively, other chromatographic columns capable of achieving similar separation performance may be used. Rinsing solution. 30 mmol/L potassium hydroxide solution. Eluent flow rate.

1.0 mL/min. Column temperature. 30°C. Detector temperature. 35°C. Suppressor. Anion suppressor. Suppression current. 75mA. Injection volume. 25 µL. The above instrument conditions can be optimized according to specific circumstances. Typical ion chromatograms for the determination of chloride, sulfate and phosphate content are shown in Figure A.1 of Appendix A.

6.4.2.3 Determination Method Depending on the anion content in the sample, weigh 10g~50g (accurate to 0.0001g) of sample and place it in an evaporating dish in water. Evaporate and concentrate to approximately 5 mL on a bath or adjustable temperature hot plate. After cooling, transfer to a 100 mL volumetric flask and dilute to the mark. The determination shall be performed in accordance with the provisions of

10.5.1 in GB/T 34672-2017, and a blank test shall also be performed.

6.4.2.4 Calculation The mass fraction (w2) of anions is calculated according to formula (2).

6.5 Sulfides Take 55 mL (50

g) of sample, add

0.5 mL of lead acetate (alkaline solution), shake well, and the dark color of the solution should not be deeper than that of the standard colorimetric solution. The standard colorimetric solution is prepared by taking a solution containing

0.010 mg (high purity, analytical grade, or analytical grade) or

0.025 mg (chemically pure) of sulfide (S) standard. The standard solution was diluted to 55 mL and treated in the same way as the sample.

6.6 Sulfates

6.6.1 Turbidimetric method (excluding arbitration method - high purity) Take 10 mL (5 mL for chemically pure solutions) of the test solution (6.4.1.1), dilute to 20 mL, and acidify with

0.5 mL of 20% hydrochloric acid solution. Then, it should be determined according to GB/T 9728.The turbidity of the solution should not be greater than that of the standard turbidity solution. The standard turbidity solution is prepared by taking

0.02 mg (analytical grade),

0.04 mg (analytical grade), or

0.05 mg (chemically pure) of sulfate. (SO4) standard solution, diluted to 20 mL, was treated simultaneously with the same volume of test solution.

6.6.2 Ion Chromatography See 6.4.2.

6.7 Carbonates Take 11 mL (10

g) of sample, dilute to 40 mL with carbon dioxide-free water, add 5 mL of saturated barium hydroxide solution, shake well, and let stand. 3 min. The turbidity of the solution should not be greater than that of the standard turbidity solution. The standard turbidimetric solution is prepared by taking

0.1 mg (high-purity, analytical grade, or analytical grade) or

0.2 mg (chemically pure) carbon dioxide (CO2). The standard solution was treated in the same way as the sample.

6.8.1 Colorimetric method (excluding arbitration method - high purity) Take 5 mL (

2.5 mL for chemically pure solution) of the test solution (6.4.1.1), add 2 drops of saturated 2,4-dinitrophenol indicator solution, and add nitric acid dropwise. The solution (13%) was diluted until the yellow color just disappeared, then diluted to 10 mL and determined according to GB/T 9727.The blue color of the organic layer should not be... It is darker than the standard colorimetric solution. The standard colorimetric solution is prepared by taking

0.005 mg (analytical grade) or

0.01 mg (analytical grade, chemically pure) of phosphate (PO4) standard. The solution was diluted to 5 mL and treated simultaneously with the same volume of the test solution.

6.8.2 Ion Chromatography See 6.4.2.

6.9 Reduction of potassium permanganate Take 22 mL (20

g) of sample, add 13 mL of water, shake well, add 27 mL of sulfuric acid solution (40%) for acidification, and add

0.2 mL of potassium permanganate dropwise. Prepare a standard titration solution [c(1/5KMnO4=0.1mol/L)] and boil for 5 minutes. The pink color of the solution should not completely disappear.

6.10 Sodium, magnesium, potassium, calcium, iron, copper, lead

6.10.1 Flame atomic absorption spectrometry (excluding arbitration method - high purity)

6.10.1.1 Reagents, Materials and Instruments Comply with the provisions of Chapters 5 and 6 of GB/T 9723-2007.

6.10.1.2 Instrument Conditions Light source. Hollow cathode lamp. Wavelengths. Sodium 589.0nm, Magnesium 285.2nm, Potassium 766.5nm, Calcium 422.7nm, Iron 248.3nm, Copper 324.7nm, Lead 283.3nm. Flame. Acetylene-air.

6.10.1.3 Determination Method 6.10.1.3.1 Sodium Take

g) of sample, evaporate it to dryness in a water bath, dissolve the residue with

0.5 mL hydrochloric acid solution (15%) and an appropriate amount of water, and dilute to 50 mL. The test shall be performed in accordance with the provisions of

7.2.1 of GB/T 9723-2007, and the results shall be calculated in accordance with the provisions of

7.2.3 of GB/T 9723-2007. 6.10.1.3.2 Magnesium Take

g) of chemically pure sample], evaporate to dryness in a water bath, and rinse with

0.5 mL of hydrochloric acid solution (15%) and appropriate amount of... Dissolve the residue in water and dilute to 25 mL. Determine the concentration according to the requirements of

7.2.1 in GB/T 9723-2007, and the results shall be in accordance with GB/T 9723-2007. Calculated according to the provisions of 7.2.3. 6.10.1.3.3 Potassium Take

g) of sample, evaporate to dryness in a water bath, dissolve the residue in

0.5 mL of hydrochloric acid solution (15%) and an appropriate amount of water, and dilute to [amount missing]. 25 mL. The determination shall be made in accordance with the provisions of

7.2.1 of GB/T 9723-2007, and the results shall be calculated in accordance with the provisions of

7.2.3 of GB/T 9723-2007. 6.10.1.3.4 Calcium Take 28 mL (25

g) of chemically pure sample], evaporate to dryness in a water bath, and rinse with 1 mL of nitric acid solution (25%) and appropriate amount of... Dissolve the residue in water and dilute to 25 mL. Determine the concentration according to the requirements of

7.2.1 in GB/T 9723-2007, and the results shall be in accordance with GB/T 9723-2007. Calculated according to the provisions of 7.2.3. 6.10.1.3.5 Iron and Copper Take 44 mL (40

g) of sample [110 mL (100

6.10.2 Inductively Coupled Plasma Atomic Emission Spectrometry (except for high-purity)

6.10.2.1 Reagents, Materials and Instruments Comply with the provisions of Chapters 5 and 6 of GB/T 23942-2009.

6.10.2.2 Instrument Conditions Recommended wavelengths. Sodium 589.592nm, Magnesium 279.553nm, Potassium 766.490nm, Calcium 396.847nm, Iron 238.204nm, Copper 327.396nm, lead 220.353nm. Incident power. 1200W. Observation height. 8mm. Argon flow rate. Cooling gas

6.10.3 Inductively Coupled Plasma Mass Spectrometry

6.10.3.1 Reagents, Materials and Instruments Comply with the provisions of Chapters 5 and 6 of GB/T 39486-2020.

6.10.3.2 Instrument Conditions Ion source power. 1550W. Inlet pressure. Argon 0.5MPa~0.7MPa, Helium 0.09MPa~0.13MPa. Helium flow rate.

5.0 mL/min. Sampling depth.

10.0 mm. Atomizing gas flow rate.

1.05 L/min. Peristaltic pump.

0.10 r/min. Atomization chamber temperature. 2.0°C. Integration time. 0.3s. The above instrument conditions can be optimized according to specific circumstances.

6.10.3.3 Determination Method Weigh approximately 5g of sample and slowly pour it into a 50mL volumetric flask containing a small amount of water. Cool to room temperature, dilute to the mark, and shake well. Simultaneously... Perform a blank test. Determine the results according to section

8.4.2 of GB/T 39486-2020, and the results should conform to section

9.2 of GB/T 39486-2020. calculate.

6.11 Lithium, silver, gold, beryllium, strontium, barium, zinc, cadmium, mercury, aluminum, gallium, indium, thallium, titanium, tin, vanadium, arsenic, antimony, bismuth, chromium, molybdenum, manganese, cobalt, nickel, boron, zirconium, silicon See 6.10.3.