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GB 5009.182-2017

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GB 5009.182-2017 英文版 250 购买 现货,9秒内自动发货PDF,有增值税发票。 食品安全国家标准 食品中铝的测定 有效

   
标准编号: GB 5009.182-2017 (GB5009.182-2017)
中文名称: 食品安全国家标准 食品中铝的测定
英文名称: Food safety national standard -- Determination of aluminum in food
行业: 国家标准
中标分类: X09
字数估计: 11,117
发布日期: 2017-04-06
实施日期: 2017-10-06
旧标准 (被替代): GB/T 5009.182-2003; GB/T 23374-2009; GB/T 18932.11-2002部分; SN/T 2208-2008部分
标准依据: State Health and Family Planning Commission Notice No. 5 of 2017

GB 5009.182-2017
Food safety national standard -- Determination of aluminum in food
中华人民共和国国家标准
食品安全国家标准
食品中铝的测定
2017-04-06发布
2017-10-06实施
中华人民共和国国家卫生和计划生育委员会
国 家 食 品 药 品 监 督 管 理 总 局 发 布
前言
本标准代替GB/T 5009.182-2003《面制食品中铝的测定》、GB/T 23374-2009《食品中铝的测定
电感耦合等离子体质谱法》、GB/T 18932.11-2002《蜂蜜中钾、磷、铁、钙、锌、铝、钠、镁、硼、锰、铜、
钡、钛、钒、镍、钴、铬含量的测定方法 电感耦合等离子体原子发射光谱(ICP-AES)法》、SN/T 2208-
2008《水产品中钠、镁、铝、钙、铬、铁、镍、铜、锌、砷、锶、钼、镉、铅、汞、硒的测定 微波消解-电感耦合等
离子体质谱法》中铝的测定方法。
本标准与GB/T 5009.182-2003相比,主要变化如下.
---标准名称修改为“食品安全国家标准食品中铝的测定”;
---改进了第一法分光光度法;
---增加电感耦合等离子体质谱法为第二法;
---增加电感耦合等离子体发射光谱法为第三法;
---增加石墨炉原子吸收光谱法为第四法。
食品安全国家标准
食品中铝的测定
1 范围
本标准规定了食品中铝含量测定的分光光度法、电感耦合等离子体质谱法、电感耦合等离子体发射
光谱法和石墨炉原子吸收光谱法。
本标准第一法适用于检测使用含铝食品添加剂的食品中的铝,第二法、第三法和第四法适用于检测
食品中的铝。
第一法 分光光度法
2 原理
试样经处理后,在乙二胺-盐酸缓冲液中(pH6.7~7.0),聚乙二醇辛基苯醚(TritonX-100)和溴代
十六烷基吡啶(CPB)的存在下,三价铝离子与铬天青S反应生成蓝绿色的四元胶束,于620nm波长处
测定吸光度值并与标准系列比较定量。
3 试剂和材料
除非另有说明,所用试剂均为分析纯,实验用水为GB/T 6682规定的三级水。
3.1 试剂
3.1.1 硝酸(HNO3).优级纯。
3.1.2 硫酸(H2SO4).优级纯。
3.1.3 盐酸(HCl).优级纯。
3.1.4 氨水(NH3·H2O).优级纯。
3.1.5 无水乙醇(C2H6O).优级纯。
3.1.6 对硝基苯酚(C6H5NO3)。
3.1.7 铬天青S(C23H13O9SCl2Na3)。
3.1.8 乙二胺(C2H8N2)。
3.1.9 聚乙二醇辛基苯醚(TritonX-100)。
3.1.10 溴代十六烷基吡啶(CPB,C21H38BrN)。
3.1.11 抗坏血酸(C6H8O6)。
3.2 试剂配制
3.2.1 盐酸溶液(1+1).量取50mL盐酸与50mL水混合均匀。
3.2.2 硫酸溶液(1%).吸取1mL硫酸缓慢加入到80mL水中,放冷后用水稀释至100mL,混匀。
3.2.3 对硝基苯酚乙醇溶液(1g/L).称取0.1g对硝基苯酚,溶于100mL无水乙醇中,混匀。
3.2.4 硝酸溶液(5%).量取5mL硝酸,加水定容至100mL,混匀。
3.2.5 硝酸溶液(2.5%).量取2.5mL硝酸,加水定容至100mL,混匀。
3.2.6 氨水溶液(1+1).量取10mL氨水,加入10mL水中,混匀。
3.2.7 硝酸溶液(2+98).量取2mL硝酸与98mL水混合均匀。
3.2.8 乙醇溶液(1+1).量取50mL无水乙醇溶于50mL水中,混匀。
3.2.9 铬天青S溶液(1g/L).称取0.1g铬天青S溶于100mL乙醇溶液(1+1)中,混匀。
3.2.10 TritonX-100溶液(3%).吸取3mLTritonX-100置于100mL容量瓶中,加水定容至刻度,
混匀。
3.2.11 CPB溶液(3g/L).称取0.3gCPB溶于15mL无水乙醇中,加水稀释至100mL,混匀。
3.2.12 乙二胺溶液(1+2).量取10mL乙二胺缓慢加入20mL水中,混匀。
3.2.13 乙二胺-盐酸缓冲溶液(pH6.7~7.0).量取100mL乙二胺沿玻璃棒缓慢加入200mL水中,待
冷却后再沿玻璃棒缓缓加入190mL盐酸,混匀,若pH>7.0或pH<6.7时可分别用盐酸溶液(1+1)或
乙二胺溶液(1+2)调节pH。
3.2.14 抗坏血酸溶液(10g/L).称取1g抗坏血酸,用水溶解并定容至100mL,混匀。临用时现配。
3.3 标准品
铝标准溶液.1000mg/L。或经国家认证并授予标准物质证书的一定浓度的铝标准溶液。
3.4 标准溶液配制
3.4.1 铝标准中间液(100mg/L).准确吸取1.00mL铝标准溶液(1000mg/L)于10mL容量瓶中,加
硝酸溶液(5%)定容至刻度,混匀。
3.4.2 铝标准使用液(1.00mg/L).准确吸取1.00mL铝标准中间液(100mg/L),置于100mL容量瓶
中,用硝酸溶液(5%)稀释至刻度,混匀。
4 仪器和设备
注.所有玻璃仪器均需以硝酸(1+5)浸泡24h以上,用自来水反复冲洗,最后用水冲洗晾干后方可使用。
4.1 分光光度计。
4.2 天平.感量1mg。
4.3 可调式控温电热炉或电热板。
4.4 酸度计(±0.1pH)。
4.5 恒温干燥箱。
5 分析步骤
在采样和试样制备过程中,应注意不使试样污染,应避免使用含铝器具。
面制品、豆制品、虾味片、烘焙食品等样品粉碎均匀后,取约30g置85℃恒温干燥箱中干燥4h。
5.2 试样消解
称取试样0.2g~3g(精确至0.001g)或准确移取液体试样0.500mL~5.00mL,置于硬质玻璃消
化管或锥形瓶中,加入10mL硝酸,0.5mL硫酸,在可调式控温电热炉或电热板上加热,推荐条件.100℃
加热1h,升至150℃加热1h,再升至180℃加热2h,然后升至200℃,若变棕黑色,再补加硝酸消化,
直至管口冒白烟,消化液呈无色透明或略带黄色。取出冷却,用水转移定容至50mL(V1)容量瓶中,混
匀备用。同时做试剂空白试验。
5.3 显色反应及比色测定
另取25mL具塞比色管7支,分别加入铝标准使用溶液0mL、0.500mL、1.00mL、2.00mL、3.00mL、
4.00mL和5.00mL(该系列标准溶液中铝的质量分别为0μg、0.500μg、1.00μg、2.00μg、3.00μg、
4.00μg、5.00μg),并依次向各管中加入硫酸溶液(1%)1mL,加水至10mL刻度。
向标准管、试样管、试剂空白管中滴加1滴对硝基苯酚乙醇溶液(1g/L),混匀,滴加氨水溶液(1+1)
至浅黄色,滴加硝酸溶液(2.5%)至黄色刚刚消失,再多加1mL,加入1mL抗坏血酸溶液(10g/L),混
匀后加3mL铬天青S溶液(1g/L),混匀后加1mLTritonX-100溶液(3%),3mLCPB溶液(3g/L),
3mL乙二胺-盐酸缓冲溶液,加水定容至25.0mL,混匀,放置40min。
于620nm波长处,用1cm比色皿以空白溶液为参比测定吸光度值。以标准系列溶液中铝的质量
为横坐标,以相应的吸光度值为纵坐标,并绘制标准曲线。根据试样消化液的吸光度值与标准曲线比较
6 分析结果的表述
试样中铝含量按式(1)计算.
X=
(m1-m0)×V1
m×V2
(1)
式中.
X ---试样中铝的含量,单位为毫克每千克或毫克每升(mg/kg或mg/L);
m1 ---测定用试样消化液中铝的质量,单位为微克(μg);
V1 ---试样消化液总体积,单位为毫升(mL);
V2 ---测定用试样消化液体积,单位为毫升(mL);
m ---试样称样量或移取体积,单位为克或毫升(g或mL)。
计算结果保留三位有效数字。
7 精密度
在重复性条件下获得的两次独立测定结果的绝对差值不得超过算术平均值的10%。
8 其他
当称样量为1g(或1mL),定容体积为50mL时,方法的检出限为8mg/kg(或8mg/L),定量限
为25mg/kg(或25mg/L)。
见GB 5009.268。
第三法 电感耦合等离子体发射光谱法
见GB 5009.268。
第四法 石墨炉原子吸收光谱法
9 原理
试样消解处理后,经石墨炉原子化,在257.4nm处测定吸光度。在一定浓度范围内铝含量与吸光
度值成正比,与标准系列比较定量。
10 试剂和材料
除非另有说明,所用试剂为优级纯,试验用水为GB/T 6682规定的二级水。
10.1.1 硝酸(HNO3)。
10.1.2 硫酸(H2SO4)。
10.2 试剂配制
10.2.1 硝酸溶液(1+99).吸取1mL硝酸加入99mL水中,混匀。
10.2.2 硝酸溶液(5+95).量取5mL硝酸加入95mL水中,混匀。
10.3 标准品
铝标准溶液.1000mg/L。或经国家认证并授予标准物质证书的一定浓度的铝标准溶液。
10.4 标准溶液配制
10.4.1 铝标准中间液(100mg/L).准确吸取1.00mL铝标准溶液(1000mg/L)于10mL容量瓶中,
10.4.2 铝标准使用液(1.00mg/L).准确吸取1.00mL铝标准中间液(100mg/L),置于100mL容量
瓶中,用硝酸溶液(5+95)稀释至刻度,混匀后再从中准确吸取1.00mL于100mL容量瓶中,用水稀释
至刻度,混匀。
10.4.3 铝标准系列溶液.分别吸取铝标准使用液(1.00mg/L)0mL、2.50mL、5.00mL、10.0mL、
15.0mL和20.0mL于100mL容量瓶中,加硝酸溶液(1+99)至刻度,混匀。此铝标准系列溶液的质
量浓度分别为0μg/L、25.0μg/L、50.0μg/L、100μg/L、150μg/L和200μg/L。
11 仪器和设备
注.所有玻璃仪器、消解罐均需以硝酸(1+5)浸泡24h以上,用自来水反复冲洗,最后用水冲洗晾干后方可使用。
11.1 石墨炉原子吸收光谱仪.附铝空心阴极灯。
11.3 可调式控温电热炉。
11.4 可调式电热板。
11.5 微波消解仪.配聚四氟乙烯消解内罐。
11.6 压力消解罐.配聚四氟乙烯消解内罐。
11.7 恒温干燥箱。
12 分析步骤
12.1 试样制备
注.在采样和试样制备过程中,应避免污染,应避免使用含铝器具。
12.1.1 粮食、豆类样品
12.1.2 蔬菜、水果、鱼类、肉类等水分含量高的样品
样品用水洗净,晾干,取可食部分,制成匀浆,储于塑料瓶中。
12.1.3 饮料、酒、醋、酱油等液体样品
将样品摇匀。
12.1.4 面制品、豆制品、虾味片、烘焙食品等样品
样品粉碎均匀后,取约30g置85℃恒温干燥箱中干燥4h。
12.2 试样消解
12.2.1 湿法消解
称取固体试样0.2g~3g(精确至0.001g)或准确移取液体试样0.500mL~5.00mL,置于硬质玻
至150℃加热1h,再升至180℃加热2h,然后升至200℃,若变棕黑色,再补加硝酸消化。直至管口冒
白烟,消化液呈无色透明或略带黄色。取出冷却,用水转移定容至25mL容量瓶,混匀备用,同时做试
剂空白试验。亦可采用锥形瓶,于可调式电热板上,按上述操作方法进行湿式消解。
12.2.2 微波消解
称取固体试样0.2g~0.8g(精确至0.001g)或准确移取液体试样0.500mL~3.00mL,置于微波
消解内罐中,加入硝酸5mL~8mL,盖上内罐盖,然后旋紧外盖置于微波消解仪中,根据不同种类的试
样设置微波炉消解系统的消解条件(具体消解条件参考附录A),消解完毕待消解罐冷却至室温后,打开
消解罐,于电热板上赶酸至近干,待降至室温后用少许水洗涤消化罐3次~4次,洗液合并于25mL容
量瓶中,用水定容至刻度,混匀备用,同时做试剂空白试验。
称取固体试样0.2g~1g(精确至0.001g)或准确移取液体试样0.500mL~5.00mL,置于压力消
解内罐中,加入硝酸5mL~8mL,盖上内盖,旋紧外套,置于恒温干燥箱中,消解完毕待消解罐冷却至室温
后,打开压力消解罐,取出内罐,在电热板上赶酸至近干,待降至室温后用少许水洗涤消化罐3次~4次,
洗液合并于25mL容量瓶中,用水定容至刻度,混匀备用,同时做试剂空白试验(具体消解条件参考附
录B)。
12.3 测定
12.3.1 仪器参考条件
根据各自仪器性能调至最佳状态。参考条件为波长257.4nm,狭缝0.5nm,灯电流10mA~
15mA,干燥温度85℃~120℃,30s;灰化温度1000℃~1200℃,持续15s~20s,原子化温度
12.3.2 标准曲线制作
按质量浓度由低到高的顺序将10μL标准系列溶液(可根据使用仪器选择最佳进样量)注入石墨
管,原子化后测其吸光度值。以质量浓度为横坐标,吸光度值为纵坐标,制作标准曲线。
12.3.3 试样溶液的测定
按仪器最佳进样量将适当体积的试样消化液、空白溶液分别注入石墨炉中,测定其吸光度值,由标
准曲线得到试样消化液中中铝的质量浓度。
13 分析结果的表述
试样中铝的含量按式(2)计算.
X=
m×1000
(2)
式中.
X ---试样中铝的含量,单位为毫克每千克或毫克每升(mg/kg或mg/L);
ρ ---试样溶液中铝的质量浓度,单位为微克每升(μg/L);
ρ0 ---空白溶液中铝的质量浓度,单位为微克每升(μg/L);
m ---试样称样量或移取体积,单位为克或毫升(g或mL);
V ---试样消化液的定容体积,单位为毫升(mL);
1000---换算系数。
当铝含量≥10mg/kg(mg/L)时,计算结果保留三位有效数字;当铝含量<10mg/kg(mg/L)时,计
算结果保留两位有效数字。
14 精密度
在重复性条件下获得的两次独立测定结果的绝对差值不得超过算术平均值的20%。
15 其他
当称样量为0.5g(或0.5mL),定容体积为25mL时,方法的检出限为0.3mg/kg(或0.3mg/L),
定量限为0.8mg/kg(或0.8mg/L)。
附 录 A
微波消解升温程序
表A.1 微波消解升温程序
步骤
控制温度
升温时间
min
恒温时间
min
附 录 B
压力罐消解参考加热条件
表B.1 压力罐消解参考加热条件
步骤
温度
保持时间

GB 5009.182-2017
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National food safety standard -
Determination of aluminum in foods
食品安全国家标准
食品中铝的测定
ISSUED ON. APRIL 6, 2017
IMPLEMENTED ON. OCTOBER 6, 2017
Issued by. National Health and Family Planning Commission of the PRC;
China Food and Drug Administration.
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Table of Contents
Foreword ... 3 
1 Scope .. 4 
2 Principles ... 4 
3 Reagents and materials .. 4 
4 Instrument and equipment .. 6 
5 Analytical procedures ... 7 
6 Analysis results expression ... 8 
7 Precision... 8 
8 Others ... 8 
9 Principles ... 9 
10 Reagents and materials... 9 
11 Instrument and equipment ... 10 
12 Analytical procedures .. 10 
13 Analysis results expression .. 13 
14 Precision .. 13 
15 Others ... 13 
Appendix A Microwave digestion temperature-rise program ... 14 
Appendix B Pressure-tank digestion reference heating conditions .. 15 
Foreword
For the determination method of aluminum, this standard replaces GB/T
5009.182-2003 “Determination of aluminum in flour products”, GB/T 23374-
2009 “Determination of aluminium in foods - Inductively coupled plasma mass
spectrometry”, GB/T 18932.11-2002 “Method for the determination of
potassium, phosphorus, iron, calcium, zinc, aluminium, sodium, magnesium,
boron, manganese, copper, barium, titanium, vanadium, nickel, cobalt,
chromium contents in honey. Inductively coupled plasma atomic emission
spectrometric method (ICP-AES)”, SN/T 2208-2008 “Determination of sodium,
magnesium, aluminium, calcium, chromium, iron, nickel, copper, zinc, arsenic,
strontium, molybdenum, cadmium, lead, mercury, selenium, in aquatic products
- Microwave digestion - ICP/MS method ".
As compared with GB/T 5009.182-2003, the main changes of this standard are
as follows.
---The standard name is changed to “National food safety standard -
Determination of aluminium in foods";
---Improve method I spectrophotometry;
---Add inductively coupled plasma mass spectrometry as method II;
---Add inductively coupled plasma emission spectrometry as method III;
---Add graphite furnace atomic absorption spectrometry as method IV.
National food safety standard -
Determination of aluminum in foods
1 Scope
This standard specifies some methods for determination of aluminum content
in foods, such as spectrophotometry, inductively coupled plasma mass
spectrometry, inductively coupled plasma emission spectrometry and graphite
furnace atomic absorption spectrometry.
Method I in this standard applies to the detection of aluminum in foods
containing aluminum-based food additives. Method II, method III and method
IV are applicable to the detection of aluminum in foods.
Method I. Spectrophotometry
2 Principles
After the sample is treated, it is in ethylenediamine-HCl buffer solution (pH 6.7-
7.0), with the existence of Triton X-100 and cetylpyridinium bromide (CPB),
trivalence aluminum ion reacts with chrome azurol S to generate blue-green
nm and compared with the standard series for quantitation.
3 Reagents and materials
Unless otherwise indicated, the reagents used in this method are analytical
pure, the experimental water is the grade-3 water specified in GB/T 6682.
3.1 Reagents
3.1.1 Nitric acid (HNO3). guaranteed reagent.
3.1.2 Sulfuric acid (H2SO4). guaranteed reagent.
3.1.3 Hydrochloric acid (HCl). guaranteed reagent.
3.1.4 Ammonium hydroxide (NH3 • H2O). guaranteed reagent.
3.1.6 P-nitrophenol (C6H5NO3).
3.1.7 Chrome azurol S (C23H13O9SCl2Na3).
3.1.8 Ethylenediamine (C2H8N2).
3.1.9 Polyethylene glycol octyl phenyl ether (Triton X-100).
3.1.10 Cetylpyridinium bromide (CPB, C21H38BrN).
3.1.11 Ascorbic acid (C6H8O6).
3.2 Reagent preparation
3.2.1 Hydrochloric acid solution (1+1). MEASURE 50 mL of hydrochloric acid;
MIX it uniformly with 50 mL of water.
into 80 mL of water; USE water to dilute it to 100 ml after cooling; MIX it
uniformly.
3.2.3 P-nitrophenol ethanol solution (1 g/L). WEIGH 0.1 g of p-nitrophenol;
DISSOLVE it in 100 mL of anhydrous ethanol; MIX it uniformly.
3.2.4 Nitric acid solution (5%). MEASURE 5 mL of nitric acid; ADD water to
dilute it to 100 mL; MIX it uniformly.
3.2.5 Nitric acid solution (2.5%). MEASURE 2.5 mL of nitric acid; ADD water to
dilute it to 100 mL; MIX it uniformly.
3.2.6 Ammonium hydroxide solution (1+1). MEASURE 10 mL of ammonium
3.2.7 Nitric acid solution (2+98). MEASURE 2 mL of nitric acid; MIX it uniformly
with 98 mL of water.
3.2.8 Ethanol solution (1+1). MEASURE 50 mL of anhydrous ethanol;
DISSOLVE it in 50 mL of water; MIX it uniformly.
3.2.9 Chrome azurol S solution (1 g/L). WEIGH 0.1 g of chrome azurol S;
DISSOLVE it in 100 mL of ethanol solution (1+1); MIX it uniformly.
3.2.10 TritonX-100 solution (3%). PIPETTE 3 mL of TritonX-100; PLACE it into
100 mL volumetric flask; ADD water to dilute it to the mark; MIX it uniformly.
3.2.11 CPB solution (3 g/L). WEIGH 0.3 g of CPB; DISSOLVE it in 15 mL of
5 Analytical procedures
5.1 Sample Preparation
In the process of sampling and sample preparation, pay attention not to
contaminate the sample; avoid using aluminum-containing appliances.
After crushing the samples of flour products, bean products, shrimp flavorings
and bakery products uniformly, TAKE out 30 g of sample; PLACE it into
constant-temperature oven at 85°C for 4h.
5.2 Sample digestion
WEIGH 0.2 g ~ 3 g of sample (accurate to 0.001g) or accurately MOVE 0.500
ADD 10 mL of nitric acid and 0.5 mL of sulfuric acid; HEAT it on adjustable
temperature-control electric furnace or hot plate, reference conditions. heat it at
100°C for 1h; rise to 150°C and heat it for 1h; rise to 180°C and heat it for 2h;
then rise to 200°C. If it becomes brownish black, ADD nitric acid again to digest;
until the tube mouth emits white smoke, digestive juice is colorless and
transparent or slightly yellow. TAKE it out; after cooling, USE water to transfer
and dilute it to 50 mL (V1) volumetric flask; MIX it uniformly for spare-use.
Meanwhile, DO a reagent blank test.
5.3 Color reaction and colorimetric determination
solution; PLACE them into 25 mL plugged colorimetric tube; ADD water to 10
mL. In addition, TAKE seven 25 mL plugged colorimetric tubes; ADD
respectively aluminum standard working solution 0 mL, 0.500 mL, 1.00 mL,
2.00 mL, 3.00 mL, 4.00 mL and 5.00 mL (in the series standard solution, the
mass of aluminum is 0 μg, 0.500 μg, 1.00 μg, 2.00 μg, 3.00 μg, 4.00 μg, 5.00
μg respectively); ADD 1 mL of sulfuric acid solution (1%) in each tube
successively; ADD water to 10 mL.
ADD dropwise 1 drop of p-nitrophenol ethanol solution (1 g/L) into standard
tube, sample tube and reagent blank tube; MIX it uniformly; ADD dropwise
dropwise nitric acid solution (2.5%) until the yellow just disappears; ADD again
1 mL of nitric acid solution; ADD 1 mL of ascorbic acid solution (10 g/L); after
mixing it uniformly, ADD 3 mL of chrome azurol S solution (1 g/L); after mixing
it uniformly, ADD 1 mL of TritonX-100 solution (3%), 3 mL of CPB solution (3
g/L), 3 mL of ethylenediamine - hydrochloric acid buffer solution; ADD water to
dilute it to 25.0 mL; MIX it uniformly; PLACE it for 40min.
10.4 Standard solution preparation
10.4.1 Aluminum standard intermediate solution (100 mg/L). Accurately
PIPETTE 1.00 mL of aluminum standard solution (1000 mg/L) into 10 mL
uniformly.
10.4.2 Aluminum standard working solution (1.00 mg/L). Accurately PIPETTE
1.00 mL of aluminum standard intermediate solution (100 mg/L) into 100 mL
volumetric flask; USE nitric acid solution (5 + 95) to dilute it to the mark; after
mixing it uniformly, PIPETTE accurately 1.00 mL from the solution; PLACE it
into 100 mL volumetric flask; USE water to dilute it to the mark; MIX it uniformly.
10.4.3 Aluminum standard series solution. PIPETTE respectively aluminum
standard solution (1.00 mg / L) 0 mL, 2.50 mL, 5.00 mL, 10.0 mL, 15.0 mL and
20.0 mL into 100 mL volumetric flask; ADD nitric acid solution (1+99) to the
solution is 0 μg/L, 25.0 μg/L, 50.0 μg/L, 100 μg/L, 150 μg/L and 200 μg/L
respectively.
11 Instrument and equipment
Note. All glassware and digestion pots must be soaked in nitric acid solution
(1+5) for more than 24h, washed repeatedly with tap water, finally rinsed with
water. Dry it by airing before use.
11.1 Graphite Furnace Atomic Absorption Spectrometer. Attached aluminum
hollow cathode lamp.
11.2 Balance. sensitivity is 1 mg.
11.4 Adjustable hot plate.
11.5 Microwave digestion instrument. equipped with Teflon digestion inner-tank.
11.6 Pressure digestion pot. equipped with Teflon digestion inner-tank.
11.7 Constant-temperature oven
12 Analytical procedures
12.1 Sample preparation
temperature, OPEN the digestion tank; CATCH-acid to dry on electric hot plate;
when it is reduced to room temperature, USE a small amount of water to wash
the digestion tank for 3~4 times; COMBINE washing liquid in 25 mL volumetric
Meanwhile, DO a sample blank test.
12.2.3 Pressure-tank digestion
WEIGH 0.2 g ~ 1 g of solid sample (accurate to 0.001 g) or accurately MOVE
0.500 mL ~ 5.00 mL of liquid sample into pressure digestion inner-tank; ADD 5
mL~ 8mL of nitric acid; COVER inner-cap; TIGHTEN outer-sheath; PLACE it
into constant-temperature oven; after digestion tank is cooled to room
temperature, OPEN the pressure digestion tank; TAKE out inner-tank; CATCH-
acid to dry on electric hot plate; when it is reduced to room temperature, USE
a small amount of water to wash the digestion tank for 3~4 times; COMBINE
it uniformly for spare-use. Meanwhile, DO a sample blank test. (specific
digestion conditions refer to Appendix B).
12.3 Determination
12.3.1 Instrument’s test conditions
Adjust to optimum state according to performance of each instrument. The
reference conditions are a wavelength of 257.4 nm, a slit of 0.5 nm, a lamp
current of 10 mA ~ 15 mA, a drying temperature of 85° C. ~ 120° C. for 30 s; an
ashing temperature of 1000° C. ~ 1200° C. for 15 s to 20 s; an atomization
temperature of 2750° C. for 4s ~ 5s; internal gas flow 0.3 L/min, the injection
   
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