甲基苯并三氮唑(TTA)检验方法
THE TEST METHOD FOR TOLYLTRIAZOLE
1、方法概要
1.Method and Summary
把试样溶于蒸馏水中，加入适量硝酸银溶液，搅拌生成白沉淀物，用已恒重的微孔玻璃器过滤，烘干至恒重，以所得沉淀物质量计算试样纯度。
Put the sample into the DI water,add silver nitrate solution,whip to white settling,filter with the micro-aperture weighted volumetric glass,dry to permanent weight,calculate the sample purity as the quality of the settling.
2、仪器和试剂
2.Instrument and Reagent
2.1、微孔玻璃器：坩埚，1G3；
2.1.Micro-aperture volumetric glass:Cauldron，1G3；
2.2、烧杯：300ml，500ml；
2.2.Beaker:300ml，500ml；
2.3、吸滤瓶：1000ml；
2.3.Filter flask:1000ml;
2.4、试验用小型真空泵；
2.4.Little vacuum pump tested;
2.5、天平：分值度为0.1mg
2.5.Balance:Scale Division 0.1mg
2.6、天平：分值度为0.1mg；
2.6.Balance:Scale Division 0.1mg
2.7、稀氨水、浓氨水：蒸馏=1：99体积比；
2.7.Aqua ammoniae,Stronger Ammonia Water:Distillation=1:99 Volume Ratio
2.8、硝酸银：分析纯，配成10%水溶液。
2.8.Silver nitrate:Analytically pure,Blending to 10%water solution.
3、试验步骤
3.The test process
3.1、把微孔玻璃器洗干净，在110℃烘干箱中干燥3h后取出放入干燥器中，冷却30min后称重，称准至0.00002g，重复烘干，冷却及称重，直至连续间称重差数不大于0.0004g为止。
3.1.Clean the micro-aperture volumetric glass,dry for 3h when the temperture 110℃in the l for 30min,then weigh to 0.00002g,repeat dry,cool and weigh.until the weight margin not bigger than 0.0004g.
3.2、称重试样0.4500-0.5000，溶于150ml蒸馏水中。
3.2.Weigh sample 0.4500-0.5000,dissolve in 150ml DI water.
3.3、在3.2中加入浓氨水8ml，用中速定量滤纸过滤，取8ml稀氨水冲浇3次。
3.3.Put 8ml stronger Ammonia Water in to 3.2.filter with the medium speed ration filter paper,flushing 3 times with 8ml aqua ammoniae.
3.4、在3.3的滤液中边搅拌边连续加入8ml 10%硝酸银水溶液，搅拌30min，得白沉淀物。
3.4.In the 3.3 filtrate,whip while add 8ml 10%silver nitrate water solution,filter for 30 min to the white settling.
3.5、用3.1已恒重的微孔玻璃器过滤3.4所设的白沉淀物，并用稀氨水30ml冲洗6次，用真空泵抽干。
3.5.Use the 3.1 micro-aperture volumetric glass filter the 3.4 white settling,and use the 30ml aqua ammoniae to flush for 6 times.Then swab-off with the vacuum pump.
3.6、将盛有白沉淀物的微孔玻璃器放入110℃的烘箱中干燥3h，冷却、称重，并恒重至00
002g。
3.6.Put the micro-aperture volumetric glass which have the white settling in to the 110℃drying case to dry for 3h,cool then weigh until the weight to 00002g.
4、计算
4.Calculate
试样的纯度X%（m/n）按式（1）计算：
The Purity for the sample X%(m/n)according to(1)
（G2-G0）×0.5470
X=————————×100……………(1)
G1
式中：G1—样品质量，g；
G1 the quality for the sample,g;
G2—沉淀物和微孔玻璃器质量，g；
G2 the quality for the settling and micro-aperture volumetric glass,g
G3—微孔玻璃器质量，g；
G3 the quality for the micro-aperture volumetric glass,g;
0.5470—样品沉淀物与样品间的转换系数。
0.5470 internal conversion coefficient between the settling and the sample
5、精密度
5.Precision
两个平行测定结果之间的差值不应大于平均值的0.4%。
The D-value for the two parallel test result should not bigger than 0.4%of the average value
甲基苯骈三氮唑熔点测定方法
THEweight和weigh的转换 TEST METHOD FOR MELTING POINT IN TTA
1.仪器、试剂
1.Instrument and Reagent
1.1圆底烧瓶：250ml,直径80mm,颈长20-30mm,口径30mm；
1.1.Round flask:250ml,diameter 80mm,neck length:20-30mm,caliber30mm
1.2内标式单球温度计:分度值0.1℃；
1.2.Enclosed-scale Single ball thermometer:division value 0.1℃
1.3.辅助温度计:分度值1℃；
1.3.Auxiliary thermometer:division value 1℃
1.4.培养皿；
1.4.Culture dish
1.5.毛细管；
1.5.Capillary tube
1.6.玻璃棒；
1.6.Glass rod
1.7.胶塞:外侧有出气槽；
1.7.Parting lock:with outlet gaps offside
1.8.液体石蜡；
1.8.Liquid paraffin
1.9.调压电炉:1000W；
1.9.Pressure regulation electric cooker:100W
1.10.试管
1.10.Test tube
1、操作步骤
2.Test process
2.1、取苯骈三氮唑样品少许，放入培养皿中，用玻璃棒轻轻搅细碎；
2.1.Put a little benzotriazole sample into the capillary tube,whip thin and smash with the glass rod gently
2.2、取一根毛细管，装入2-3mm样品至管底；
2.2.Put 2-3mm sample into the bottom of the capillary tube;
2.3、将毛细管粘住烧瓶内标单球温度计上,烧瓶内盛3/4的石蜡液,孔处附有橡胶塞,塞上插有单球温度计,1/2单球温度计处附有辅助温度计,置电炉上加热,(注意调节电压加热)；
2.3 Putting the capillary tube stick to the single standard ball thermometer in the flask which filled 3/4 of the liquid paraffin,the hole with a rubber plug with a single ball thermometer,1/2 ball single thermomter with assitant thermometer,then into electric furnace to heat(paying attention to the voltage regulator heat)
2.4、见苯骈三氮唑开始融化,并伴有小液滴时,记下初熔点,全部融化时,记下终熔点。
2.4 Writing down the beginning and end of the melting ponit when benzotriazole bengan to melt accompanied by small droplets and melt totally.
2.5、结果表示
2.5 the results are denoted that:
熔点按式(2.1)和(2.2)计算:the melting point is calculated according to(2.1)and(2.2)
熔点=t1+Δt…………………………………(2.1)