GB/T 43753.2-2024Methods for chemical analysis of precious metals alloys electroplating wastewater - Part 2: Determination of zinc, manganese, chromium, cadmium, lead, iron, aluminium, nickel, copper and beryllium contents - Inductively coupled plasma atomic emission spectrometry (English PDF)

Foreword

This document was issued on 15 March 2024 by the State Administration for Market Regulation; Standardization Administration of the PRC and takes effect on 1 October 2024.

It is a GB/T standard: recommended rather than compulsory, but it is the text a Chinese reviewer applies when assessing a submission.

1 Scope

GB/T 43753.2-2024 is Part 2 of the Chinese analytical series for the wastewater of precious metal alloy electroplating and electroforming, and determines zinc, manganese, chromium, cadmium, lead, iron, aluminium, nickel, copper and beryllium by inductively coupled plasma atomic emission spectrometry. The matrix is the difficulty: plating effluent carries high and variable dissolved salt, complexing agents and sometimes cyanide, and the ten elements sought span four orders of magnitude in concentration, so the spectral line has to be chosen against interference rather than for sensitivity alone. The standard sets the principle, the reagents and materials, the instruments, the samples and their handling, the test procedure, the processing of the experimental data, the precision and the test report, with informative annexes giving the recommended analytical wavelengths and instrument operating parameters and the original precision test data. It took effect on 1 October 2024.

This document describes a method for determining the contents of zinc, manganese,

chromium, cadmium, lead, iron, aluminum, nickel, copper, and beryllium in wastewater

from electroplating and electroforming of precious metal alloys using inductively

coupled plasma atomic emission spectrometry.

This document applies to the determination of zinc, manganese, chromium, cadmium,

lead, iron, aluminum, nickel, copper, and beryllium contents in wastewater from

precious metal alloy electroplating and electroforming. The determination range for

zinc, manganese, chromium, cadmium, lead, iron, aluminum, nickel, copper, and

beryllium is 0.0001 mg/mL~0.1000 mg/mL.

2 Normative references

The provisions of the following documents constitute the essential clauses of this

document through normative references in this text. Among them, for any dated

reference, only the version corresponding to that date applies to this document; for any

undated reference, the latest version (including all amendments) applies to this

document.

GB/T 6682 Water for analytical laboratory use - Specification and test methods

3 Terms and definitions

This document does not contain any terms or definitions that need to be defined.

4 Principle

After the organic matter in the test specimen is digested with perchloric acid, it is

dissolved in a mixed acid. The contents of zinc, manganese, chromium, cadmium, lead,

iron, aluminum, nickel, copper and beryllium are determined by inductively coupled

plasma atomic emission spectrometry in the mixed acid medium.

5 Reagents and materials

Unless otherwise specified, only reagents confirmed to be of analytical grade shall be

used in the analysis.

5.1 Water, GB/T 6682, Grade II.

5.2 Perchloric acid (rho=1.76 g/mL).

5.3 Nitric acid (rho=1.42 g/mL).

5.4 Hydrochloric acid (rho=1.18 g/mL).

5.5 Hydrogen peroxide (rho=1.11 g/mL)

5.6 Nitric acid (1+1).

5.7 Hydrochloric acid (1+1).

5.8 Mixed acid (1+3+4). Mix 1 volume of nitric acid (5.3), 3 volumes of hydrochloric

acid (5.4) and 4 volumes of water (5.1) thoroughly, and prepare fresh before use.

5.9 Zinc standard stock solution. Weigh 0.1000 g of metallic zinc (wZn>=99.99%) and

place it in a 100 mL PTFE beaker. Add 20 mL of nitric acid (5.6), heat to dissolve,

remove nitrogen oxides, cool to room temperature, transfer to a 100 mL plastic

volumetric flask, and dilute to the mark with water (5.1). Mix well. 1 mL of this solution

contains 1 mg of zinc.

5.10 Manganese standard stock solution. Weigh 0.1000 g of metallic manganese

(wMn>=99.99%) and place it in a 100 mL PTFE beaker. Add 20 mL of nitric acid (5.6),

heat to dissolve, remove nitrogen oxides, cool to room temperature, transfer to a 100

mL plastic volumetric flask, dilute to the mark with water (5.1), and mix well. 1 mL of

this solution contains 1 mg of manganese.

5.11 Chromium standard stock solution. Weigh 0.1000 g of metallic chromium

(wCr>=99.99%) and place it in a 100 mL PTFE beaker. Add 1 mL of nitric acid (5.6) and

5 mL of hydrochloric acid (5.7). Cover with a PTFE beaker lid, heat to dissolve, transfer

to a 100 mL plastic volumetric flask, add 10 mL of hydrochloric acid (5.7), and dilute

to the mark with water (5.1). Mix well. 1 mL of this solution contains 1 mg of chromium.

5.12 Cadmium standard stock solution. Weigh 0.1000 g of metallic cadmium

(wCd>=99.99%) and place it in a 100 mL PTFE beaker. Add 20 mL of nitric acid (5.6),

heat to dissolve, remove nitrogen oxides, cool to room temperature, transfer to a 100

mL plastic volumetric flask, and dilute to the mark with water (5.1). Mix well. 1 mL of

this solution contains 1 mg of cadmium.

5.13 Lead standard stock solution. Weigh 0.1000 g of metallic lead (wPb>=99.99%) and

place it in a 100 mL PTFE beaker. Add 20 mL of nitric acid (5.6), heat to dissolve,

remove nitrogen oxides, cool to room temperature, transfer to a 100 mL plastic

volumetric flask, and dilute to the mark with water (5.1). Mix well. 1 mL of this solution

contains 1 mg of lead.

5.14 Iron standard stock solution. Weigh 0.1000 g of metallic iron (wFe>=99.99%) and

place it in a 100 mL PTFE beaker. Add 20 mL of nitric acid (5.6), heat to dissolve,

remove nitrogen oxides, cool to room temperature, transfer to a 100 mL plastic

volumetric flask, and dilute to the mark with water (5.1). Mix well. 1 mL of this solution

contains 1 mg of iron.

5.15 Aluminum standard stock solution. Weigh 0.1000 g of metallic aluminum

(wAl>=99.99%) and place it in a 100 mL PTFE beaker. Add 20 mL of hydrochloric acid

(5.7), heat to dissolve, cool to room temperature, transfer to a 100 mL plastic volumetric

flask using hydrochloric acid (5.7), dilute to the mark with water (5.1), and mix well. 1

mL of this solution contains 1 mg of aluminum.

5.16 Nickel standard stock solution. Weigh 0.1000 g of metallic nickel (wNi>=99.99%)

and place it in a 100 mL PTFE beaker. Add 20 mL of nitric acid (5.6), heat to dissolve,

remove nitrogen oxides, cool to room temperature, transfer to a 100 mL plastic

volumetric flask, and dilute to the mark with water (5.1). Mix well. 1 mL of this solution

contains 1 mg of nickel.

5.17 Copper standard stock solution. Weigh 0.1000 g of metallic copper (wCu>=99.99%)

and place it in a 100 mL PTFE beaker. Add 20 mL of nitric acid (5.6), heat to dissolve,

remove nitrogen oxides, cool to room temperature, transfer to a 100 mL plastic

volumetric flask, dilute to the mark with water (5.1), and mix well. 1 mL of this solution

contains 1 mg of copper.

5.18 Beryllium standard stock solution. Weigh 0.1000 g of metallic beryllium

(wBe>=99.95%) and place it in a 100 mL PTFE beaker. Add 20 mL of hydrochloric acid

(5.7), heat until dissolved, cool to room temperature, transfer to a 100 mL volumetric

flask, and dilute to the mark with water (5.1). Mix well. 1 mL of this solution contains

1 mg of beryllium.

5.19 Mixed standard solution of zinc, manganese, chromium, cadmium, lead, iron,

aluminum, nickel, copper, and beryllium. Add 30 mL of hydrochloric acid (5.4) to a

200 mL plastic volumetric flask, transfer 2.00 mL of the standard stock solutions

(5.9~5.18) each to the flask, dilute to the mark with water (5.1), and mix well. 1 mL of

this solution contains 10 ug each of zinc, manganese, chromium, cadmium, lead, iron,

aluminum, nickel, copper, and beryllium.

5.20 Argon (volume fraction>=99.99%).

6 Instruments and equipment

Inductively coupled plasma atomic emission spectrometer. Under optimal operating

conditions, any instrument meeting the following specifications can be used.

a) Light source. Argon plasma light source, and the maximum output power of

the emitter shall not be less than 1.3 kW.

b) Resolution. The optical resolution at around 200 nm is no greater than 0.010

nm; the optical resolution at around 400 nm is no greater than 0.020 nm.

c) Instrument stability. The instrument's stability (RSD) within 1 hour is no

greater than 2.0%.

d) Recommended operating parameters for the inductively coupled plasma

atomic emission spectrometer are given in Appendix A.

7 Samples

The samples are stored in plastic bottles for later use.

8 Test procedure

8.1 Test specimens

Transfer the sample accurately as shown in Table 1.

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