HJ Environmental Protection Standard of the People s Republic of China

Transcription

1 Translated English of Chinese Standard: HJ Translated by: Wayne Zheng et al. Environmental Protection Standard of the People s Republic of China HJ Determination of Platinum, Palladium and Rhodium Loading in the Vehicle-used Ceramic Catalytic Converters Inductive Coupled Plasma-optical Emission Spectrometry and Inductive Coupled Plasma-mass Spectrometry 车用陶瓷催化转化器中铂 钯 铑的测定 电感耦合等离子体发射光谱法和电感耦合等离子 体质谱法 Issue on: November 2, 2009 Implemented on: January 1, 2010 Issued by: Ministry of Environmental Protection 1

2 Announcement of Ministry of Environmental Protection of the People s Republic of China [2009] No. 57 To implement the Environmental Protection Law of the People s Republic of China, protect the environment and guarantee the human health, Determination of Platinum, Palladium and Rhodium Loading in the Vehicle-used Ceramic Catalytic Converters Inductive Coupled Plasma-optical Emission Spectrometry and Inductive Coupled Plasma-mass Spectrometry is approved as a professional standard and promulgated hereby. The name and serial number of this standard are as follows: Determination of Platinum, Palladium and Rhodium Loading in the Vehicle-used Ceramic Catalytic Converters Inductive Coupled Plasma-optical Emission Spectrometry and Inductive Coupled Plasma- mass Spectrometry HJ This standard is implemented as from January 1, 2010 and published by China Environmental Science Press. Its specific content is available on the official website of the Ministry of Environmental Protection (bz.mep.gov.cn). Hereby it is announced. November 3,

3 Table of Contents Foreword Application Scope Normative References Terms and Definitions Methods and Principles Reagents and Materials Instruments and Equipments Test Sample Preparation Analysis Procedures Result Calculation Precision and Accuracy Quality Assurance and Control References and Original Chinese Documents

4 Foreword This standard is formulated with a view to implementing the Environmental Protection Law of the People s Republic of China and the Law on Prevention of Air Pollution of the People s Republic of China, protecting the environment, guaranteeing the human health, controlling the emission of motor vehicles, and regulating the determination methods of platinum (Pt), palladium (Pd) and rhodium (Rh) loading in vehicle-used ceramic catalytic converters. This standard specifies inductive coupled plasma-optical emission spectrometry (ICP-OES) and inductive coupled plasma-mass spectrometry (ICP-MS) for the determination of Pt, Pd and Rh loading in the vehicle-used ceramic catalytic converters. This standard is issued for the first time. This standard was organized and formulated by the Department of Science, Technology and Standards of Ministry of Environmental Protection. Chief drafting organizations of this standard: China Automotive Technology & Research Center and Tianjin SwARC Automotive Research Laboratory Co., Ltd. Participating drafting organizations of this standard: Chinese Research Academy of Environmental Science, Kunming Sino-Platinum Metals Catalyst Co., Ltd., BASF Catalyst (Shanghai) Co., Ltd., Johnson Matthey (Shanghai) Chemicals Limited, Umicore Autocat (Suzhou) Co., Ltd., Wuxi Weifu Environmental Catalysts Co., Ltd. and Tokyo Roki (Suzhou) Co., Ltd This standard was approved by the Ministry of Environmental Protection on November 3, This standard is implemented as from January 1, The Ministry of Environmental Protection is responsible for the explanation of this standard. 4

5 Determination of Platinum, Palladium and Rhodium Loading in the Vehicle-used Ceramic Catalytic Converters Inductive Coupled Plasma-optical Emission Spectrometry and Inductive Coupled Plasma-mass Spectrometry Warning: Since hydrochloric acid, nitric acid, hydrofluoric acid and perchloric acid are highly corrosive and pungent, protective devices shall be worn as required when handling any of them in fume cupboard, so as to prevent acid mist from flowing into the respiratory tract and contacting with skin or clothing. If any contact is caused due to carelessness, emergency measures shall be taken immediately. Upon detection, any residue and raffinate shall subject to safety treatment. 1 Application Scope This standard specifies inductive coupled plasma-optical emission spectrometry (ICP-OES) and inductive coupled plasma-mass spectrometry (ICP-MS) for the determination of platinum (Pt), palladium (Pd) and rhodium (Rh) loading in the vehicle-used ceramic catalytic converters. This standard is applicable to the determination of Pt, Pd and Rh loading in catalytic converters with cordierite honeycomb ceramics as the carrier and precious metal as the active constituent. Weigh 1g sample before digesting and scaling it to 100mL; then, analyze and determine, by ICP- OES, the detection limit and lower limit which are 5μg/g and 20μg/g respectively; if by ICP-MS, the detection limit and lower limit are 0.005μg/g and 0.02μg/g respectively. 2 Normative References The following normative documents contain provisions which, through reference in this text, constitute provisions of this standard. For undated references, the latest edition applies. GB/T 6679 General Rules for Sampling Solid Chemical Products GB/T 6682 Water for Analytical Laboratory Use Specification and Test Methods GB/T 8170 Rules of Rounding Off for Numerical Values & Expression and Judgment of 5

6 200 for 2h before taking out and cooling it until room temperature. 7.3 Weight the Carrier Mass Weight he catalytic converter carrier on an electronic balance (6.6), accurate to 0.01g. 7.4 Measure the Carrier Volume The volume of carriers in different shape is measured by the following three methods: a) For regular carrier (such as cylinder or runway column) Use, in different positions, a vernier caliper to measure their volume parameters respectively from twice to 4 times, and take their average to calculate the carrier volume and round off it to a 4-digit effective figure according to GB/T b) For regular carrier whose sectional area is to calculate Take three A4 papers or above with uniform texture, use a paper knife to cut the same part on A4 paper along the cross section of carrier, and then weigh, on the analytical balance, each A4 paper and the same part on the sectional area of carrier respectively, accurate to g. Then, calculate the average sectional area of carrier according to the proportional relation between the paper mass and the paper area. The relative deviation of each measurement and average shall be less than 0.5%. The carrier length is measured by a vernier caliper and the carrier volume is the product of its sectional area and length. c) For irregular carrier Seal the catalytic converter carrier with a preservative film and place it into a vessel filled with water. Then, collect the overflowed water and weigh the water mass. The carrier volume is calculated through dividing the water mass by the water density. 7.5 Crush, Grind and Split the Sample Crush the sample to about 1mm in grain size, split it once or more with a sample splitter (6.1), and then use a grinder (6.2) to grind the split sample into powder with the grain size less than 0.075mm. 10

7 samples (if any, national or professional standard samples shall be used preferentially), analyze parallel samples and monitor accuracy and precision so as to guarantee and control the analysis quality. The accuracy of standard sample analysis shall not be greater than 10%. If there is no any similar standard substance, standard addition method shall be adopted for control The relative deviation between the determined results of parallel samples shall be less than 2%; otherwise, re-inspection shall be conducted In case of new or abnormal sample matrix, inspection shall be conducted by the following methods: Dilution grade by grade If the concentration of analyte is too high, dilution shall be conducted grade by grade (after dilution, the minimum concentration shall be 10 times of the method detection limit). The relative deviation of analysis results before and after dilution shall not exceed ±1% Standard addition to matrix The standard solution of analyte in a given amount is added to the test portion for preparing the test solution together, or directly added to the digested test solution for dilution and scaling together. The recovery value shall be 94%~106% and 97%~103% of the known value respectively. The addition level must meet the following requirements: the addition level shall be equal or close to the content of corresponding to-be-tested substance in the sample, and shall not be greater than 3 times the content of the same to-be-tested substance in the sample After analyzing 10 test solutions and at the end of all analysis, one standard blank solution [nitric acid solution (5.8)] and one standard solution are inserted to monitor the drift of the standard curve Internal standard response: the analyzer shall monitor the internal standard response as well as the ratio of internal standard and the analytic element signal response throughout the sample analysis. Such information can be used to check problems caused by factors such as mass drift, error arising from addition of internal standard or concentration increase of individual internal standard caused by background in the sample. The deviation of absolute response value of any internal standard can t exceed 60%~125% of the initial response value in blank solution above standard. If such deviation is exceeded, the system shall be cleaned by nitric acid solution (5.7), and 17

8 the response value of standard blank solution shall be monitored. If the response value exceeds the monitoring limit, sample analysis shall be suspended and the drift cause shall be found out. 18

9 References and Original Chinese Documents [1] HJ Determination of Platinum,Palladium and Rhodium loading in the vehicle-used ceramic catalytic converters.inductive coupled plasma-optical emission spectrometry and inductive coupled plasma-mass spectrometry