ICS

01.040.19CCS

43湖 南省 地 方 標 準DB43/T

2306—2022微庫侖氯含量分析儀測試方法Test

method

for

microcoulometry

chlorine

analyzers2022

-

03

-

31

發布

2022

-

-

實施湖南省市場監督管理局

發

布DB43/T

2306— 前言························································································································

Ⅲ1 ·····················································································································

12 規范性引用文件······································································································13 術語和定義············································································································14 測試條件···············································································································14.1 環境條件·········································································································14.2 儀器設備和材料································································································

15 測試項目及方法······································································································25.1 升溫速度·········································································································25.2 控溫精度·········································································································25.3 控溫誤差·········································································································25.4氣體流量控制誤差·····························································································

25.5 進樣誤差·········································································································35.6 儀器重復性······································································································35.7 儀器誤差·········································································································45.8 安全性能·········································································································4附錄

A（資料性）（15～25）℃純水密度表····································································5參考文獻····················································································································

6DB43/T

2306— 本文件按照

GB/T

—2020《標準化工作導則 第

1

部分：標準化文件的結構和起草規則》的規定起草。請注意本文件的某些內容可能涉及專利。本文件的發布機構不承擔識別專利的責任。本文件由湖南省市場監督管理局提出并歸口。司、長沙富蘭德實驗分析儀器有限公司、中國檢驗認證集團湖南有限公司。本文件主要起草人：肖克、吳雙雙、董宇、周仁發、向東、魯徐、田明棋、王理、李婭、謝艷萍、蘇湘妹、姜慧、張特樂、鄒成娜、陳鵬輝、駱熙。IIIDB43/T

—1

本文件規定了微庫侖氯含量分析儀的測試項目及方法。2

規范性引用文件文件。GB

4793.1 測量、控制和實驗室用電氣設備的安全要求

第

1

部分：通用要求GB/T

15479 工業自動化儀表絕緣電阻、絕緣強度技術要求和試驗方法3

術語和定義本文件沒有需要界定的術語和定義。4

測試條件4.1 環境條件4.1.1 5～）℃，溫度變化在±5

℃以內。4.1.2環境相對濕度：≤80％。4.1.3 工作電源：

（±22）V，（50±1）Hz。4.1.4 無影響測氯儀使用的振動和電磁干擾，無含氯氣體。4.2 儀器設備和材料4.2.1 電子天平：測量范圍≥

g，分度值

0.1

。4.2.2 標準熱電偶：測量范圍（500~1300）℃，準確度為二等及以上。4.2.3 皂膜流量計：測量范圍（50~2000）mL/min，準確度為

級及以上。4.2.4 載氣：氬氣、氮氣或氦氣，純度≥99.99％，水含量≤5

mg/kg。4.2.5氧氣：純度≥％，水含量≤5

mg/kg。4.2.6 秒表：分辨力

s，日差優于±0.5

s。4.2.7 燒杯：容量≤50

。4.2.8氯成分分析標準物質：國家有證標準物質。4.2.9 絕緣電阻表：輸出電壓≥500

V，

級及以上。4.2.10 耐壓測試儀：交流電壓≥

kV，5

級及以上。DB43/T

—5

測試項目及方法5.1 升溫速度將測溫標準熱電偶從進樣口插入至其測量端與測氯儀控溫熱電偶的測量端距離為±10

處，接通

試

3

次，按公式（1）計算升溫速度。VT

（1）t式中：T

——升溫速度，單位為攝氏度每分鐘（℃/min）； ——3

次升溫時間的平均值，單位為分鐘（）。5.2控溫精度將高溫裂解爐爐溫升至設定溫度后，輸入氧氣和載氣，穩定

15

min，將測溫標準熱電偶的測量端

30

后，每隔

s

記錄一次測試溫度，連續記錄

次，按公式（2）計算控溫精度。max

min（2）式中： Tmax

——測溫標準熱電偶

20

min——測溫標準熱電偶

20

5.3

控溫誤差測試操作同

5.2，每隔

30

s

記錄一次測試溫度和測氯儀顯示的溫度，連續記錄

20

次。以測溫標準熱電偶

20

次測氯儀顯示溫度的平均值為儀器顯示溫度值，按公式（3）計算控溫誤差。

d

s

（3）式中：T

5.4 氣體流量控制誤差對流量可調節的氣體流量控制器在靠近滿量程范圍內的

％、5080％選取

3

點流量進行測試；對只有

1

個流量值的氣體流量控制器只測試該點流量，重復測試

3

次。按公式（4）計算各試驗點的誤差，取各試驗點誤差的最大值作為氣體流量控制誤差。

f

g

DB43/T

—（4）

6（5）

——蒸餾水在

t℃時的密度（見附錄

Akg/m

）。Vr

（6）——氣體流量控制誤差，單位為％；Q ——流量

3

次測試結果的算術平均值，單位為毫升每分鐘（mL/min）；Q ——氣體流量控制器示值，單位為毫升每分鐘（）；Q

——氣體流量控制器的流量上限值，單位為毫升每分鐘（mL/min）。5.5 進樣誤差在（20±5）℃的條件下，將進樣器抽吸蒸餾水至全容量，然后將水注入燒杯內稱重，按公式（5）計算進樣器的全容量測量值，重復測量

次取平均值，按公式（6）計算進樣誤差。式中： ——進樣器的全容量測量值，單位為微升（μL）；m ——蒸餾水重量，單位為克（g）；3V

VsVs式中：Vr

——進樣誤差，單位為％；V ——進樣器

10

次全容量測試結果的算術平均值，單位為微升（μL）；

——進樣器全容量標稱值，單位為微升（μL）。5.6 儀器重復性根據測氯儀的使用范圍，選取靠近滿量程

50％濃度的氯成分分析標準物質重復測試

7

次，記錄測試值。當測氯儀使用范圍小于

5

mg/L，儀器重復性用標準偏差（）表示，按公式（7儀使用范圍大于等于

5

，儀器重復性用相對標準偏差（

）表示，按公式（8）計算。

ni

i

2

（7）式中： ——儀器重復性，單位為毫克每升（mg/L）；

——單次測試值，單位為毫克每升（mg/L）； ——7

次測試結果的算術平均值，單位為毫克每升（mg/L）； ——測試次數，=7。

i

i

2r

r

（8）DB43/T

—式中：

——儀器重復性，單位為％；——單次測試值，單位為毫克每升（mg/L）； ——7

次測試結果的算術平均值，單位為毫克每升（mg/L）；——測試次數，=7。5.7 儀器誤差根據測氯儀的使用范圍，選取靠近滿量程

20％、％、80％濃度的氯成分分析標準物質，每個濃度點重復測試

3

次，記錄測試值。當測氯儀使用范圍小于

5

mg/L，儀器誤差用絕對誤差（x）表示，9

5

xr

）計算。

s（9）式中：x

——儀器誤差，單位為毫克每升（mg/L）； ——3

次測試結果的算術平均值，單位為毫克每升（mg/L）；rr

（10）

——標準物質濃度值，單位為毫克每升（mg/L）。

ss式中：xr

——儀器誤差，單位為％； ——3

次測試結果的算術平均值，單位為毫克每升（mg/L）；

——標準物質濃度值，單位為毫克每升（mg/L）。5.8 安全性能5.8.1將高溫裂解爐爐溫升至極限溫度，按

GB

4793.1

規定的方法測試。5.8.2絕緣電阻用

500

V

頭的相線與儀器接地端子之間的絕緣電阻。5.8.3 絕緣強度與機殼之間施加試驗電壓，試驗電壓由

0

V

上升到

1.5

kV，擊穿報警電流預置

5

mA，歷時

1

min，觀察是否出現擊穿或飛弧現象，然后平穩下降到零。0.00.10.20.30.40.50.60.70.80.915999.0983999.0832999.0679999.0525999.0370999.0214999.0057998.9899998.9739998.957816998.9416998.9253998.9089998.8924998.8757998.8590998.8421998.8251998.8080998.790817998.7735998.7560998.7385998.7208998.7031998.6852998.6672998.6491998.6309998.612518998.5941998.5756998.5569998.5381998.5193998.5003998.4812998.4622998.4429998.423519998.4039998.4843998.3646998.3447998.3248998.3047998.2846998.2643998.2439998.223520998.2029998.1822998.1614998.1405998.1195998.0984998.0772998.0559998.0345998.012921997.9913997.9696997.9478997.9258997.9038997.8817997.8594997.8371997.8146997.792122997.7695997.7467997.7239997.7009997.6779997.6547997.6315997.6084997.584999