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商品粮食中还原糖和非还原糖含量的测定

hBG5531—8本标准5用适商品于食中还粮糖和非还原糖含原量测定的。中铁氰化其钾主法要适用于小粉麦1。还原糖测定11.铁氰钾化法.1.1仪1器用具1.1.和.11磨口带锥塞瓶:形001lm;11...12量:50筒ml、52ml;.1.1.1移3液:5m管;l.111.4玻.璃漏斗;1.1..15管:试直1.8径2.0~cm,高1约cm8;.11.16.锅:铝作水浴沸用;1.1.1.7电炉:2000W;.111.8.丝笼铁放置:管用;试.1.1.19试管架1;1..11.0锥形瓶1:00ml;.111..11量滴定微管:m5或l01ml刻(度0.20m);l1..1.121析天分平:感量00001.g。1.12试.1.1.剂2.195%乙;醇1..1.22乙酸冲液缓:m3冰l酸、6乙.8乙酸g钠比和重18.4的酸硫4.5ml,合混用水稀后至释1000ml;1..1.2132%钨钠溶液酸1:2钨g钠N酸aW24·O22H溶O于100l水m中;11.2..041N.铁化氰钾溶液:32.9g干纯净燥的铁化氰钾44与.0碳g钠溶酸于1000lm水中; h1..2.15乙酸盐液:溶70g纯化钾和氯40g硫锌溶酸水中于再加入,002m冰l酸乙再,用水释至1稀000lm混,匀;11...261%碘化0钾溶液10:纯碘化g钾于溶010ml水,再中一加滴和氢饱氧化溶液钠;.1.217.1%粉溶淀:液1可g性溶粉淀,少量用水润湿和调后,入沸倒水10m0l,继煮沸,搅拌直续至液溶清晰;11.2..801.N硫代硫钠溶液酸按(G54B098—5《粮、油料和植物油食脂验检般一规》附则录B行进配制标定和)。.1.3操作1方法1..3.1提1样品液:精取确取粉称5样.657g于10m0l口锥磨形瓶中,用5lm乙浸湿全部试醇样再,加50入m乙酸缓冲液,摇l后匀再入加2ml钨酸溶钠,在液振器荡混上合振摇5im,取出n滤过弃,最初去几滤液,滴收集滤于干液锥净瓶中形,此液滤为即样品测定液。另一取形锥不瓶试加样,上操同,滤液作为即白液。空.11.32氧.:精确吸取样化液品5ml于管中试,精再确加入5ml铁化氰溶钾,混液合立即后将管试置铁(丝笼,每中次可时作同干样若测定品)放剧入烈腾的水浴中沸并,使管液面在沸中水面下液~43cm加,热准02inm后取出立,即用冷水迅冷却。速.11..33定滴将试:管容物倾内10入0ml锥瓶形中用2,5m乙酸盐溶l洗液荡试管一并倾入锥形瓶,加5ml10%化钾,混匀碘后立即,用01.硫N代酸钠硫滴至淡定色黄,加再1ml粉溶液淀继续滴,定直溶至液蓝消失色,记用下去硫代硫酸钠溶液积(体V1。1)..31.空白4试验:吸空取白液5ml,替样品液同代.11..23和1..3.13操,作下记耗消的代硫酸硫溶钠液体积(V)。01.14.果结计算还原含量先按公糖(式)计1出算氧样化品中“还液原”糖所需.10铁N化氰钾液体积溶V()3,根再据此积体(lm)查表1 ,即可得查试样含中还原糖以(芽麦糖算)的计百分数按公。(1)式算:…计…………………………………………………1()式中V:─0─滴空白液定消耗氰化铁溶液体钾积,m;lV1──滴样定品消耗铁氰化液溶钾液积体m,l;hV3 ──氧化样品中还原液所需糖.10N铁氰钾溶液体化积ml;,N──代硫硫酸钠液实溶当际量浓。度试双验结果许差不允过超.05%0求其平均数,即为,检结果验。验结果取检数小后点第位二。.115..10N铁化钾氰(ml)与还原含糖对量可照表查1注。还:原含量糖以芽麦糖计。算12费.氏液法1林..12仪和用器具.21.1.1古氏埚:坩52ml;1..212.滤抽:5瓶00m;l12.1.3.空泵真或泵等。水12.2.试1.2.2.1剂费林氏溶液a;碱性.酒酸铜甲液:石取酸硫铜结晶34.693g,适量水加解,加溶硫0.酸5lm,加再水至005ml用精,石棉制滤过b;.碱酒性石铜酸乙液取:石酸酒钾1钠7g3与氢氧钠5化0,加适g量溶解水稀,释至500l,用m精制棉石滤过贮存于,有具橡皮塞玻璃的内。瓶.21..2精制石棉2:用3先N酸盐将棉石泡浸~32日后,用水洗。净再加1%氢0化钠氧溶液浸2泡3日~倾去溶液,用,碱热酒石酸性铜乙浸液数小泡,时用水洗净再。以N3盐酸浸数小时,泡用水至洗不呈酸性,使成之为微的细软纤维,用水浸贮存泡于璃瓶玻内作填,充古氏埚坩用1.2。2.3.0.1N锰酸高标钾准液溶。12.2.41N.氧氢钠溶液:化取氧化氢4钠g,加溶解水至10ml。0.2.21.5硫酸溶铁:取液酸硫50g,铁加2水00ml溶解后慢,慢入硫酸加10ml,0后冷水至加000ml。1.21.2.36N盐:取盐酸酸25m,l加至水100l。1.2.3操作方法 m01N.K3/S<e(CN)Fm6lh表1原还糖% h010.0.0203.00.400.500.60.00708.0090.1.00.10112.01.03140..5101.06.710.180.102.0029.10220.2.302.402.0256.02.07.202890.3.003.130.20.3330.403.035.0367.0.83039.040.04.04.204.130.050.100.1050.2002.0.31503.0.4610.64051.0.65.0060.650.710.670.00.858.0900961.0.1.160.1111.16.111.2261.301.351.401.54.511156..111.66617.11.71.8261.881.952.02.1072.31218..252h 440.4504..60470.4.048.059005..01.525030.5.4055.056.5.7005.05.8096.006.10620..3066.406506.60.670..806.6097.007.01.2077.30.4707.50.7067.077.08790.80.0810..280.808.340.508860.2.13.3227.42.514.5722.462.70.267.8222.882.93.052.3083.153.23.228.3433.134.4735.3.6303.73.7363.73.895.9233.98.406412..148.4254.31.34484.5451.458.4.64.724.7584.854.924.95.905 h8708..0851.52.911..231.样试理:准处称确试取10~样20g放入20m5l容量瓶,中加2水00l,在m45℃水中加热浴1,h并时时振摇,时到 待冷后水至刻度,加置静后,吸澄取清液200lm于另一502ml容量瓶中,加碱性酒酸铜甲液10石m和l1N氢氧化钠液溶4ml摇匀,加,水至刻度静,置30imn,干燥滤用过滤,弃去初纸滤液,余其滤供测液还原糖定非和还糖用。原1.23.2.滴定精:密取制备的试吸样液5溶ml于0400lm烧杯中加入,性碱酒石酸甲、乙液铜25各ml盖一表,皿面置,炉电上加热,在m4in内沸腾再,沸2mi煮,趁n用铺热有石棉的氏古坩埚或垂(坩埚)融抽滤并,用6℃0热水洗涤杯烧和淀,至沉洗不液碱性为止呈将古氏。埚放坩原回400lm烧中,杯硫酸加铁溶液52l和m2水5m,用l玻棒搅,使氧化拌铜亚完全溶解以,.10N高酸锰钾标准溶液滴定至微红。同时取水50色ml,碱性加石酸铜酒甲乙、各液2m5,l试做空剂白验。试1..42果计算结当于试样相还中糖重量原氧的化亚铜量重按式(2)公计算:=(V-xV)0×7N.541……………………………………………………()2中式:x──相当于试中还原糖样量重的氧化铜亚重量的mg;,V──试样消高耗锰钾标酸准溶的液体,m积l;V──0样试空消耗高白酸锰钾标溶液准的体,积l;mN──高锰酸钾标溶液的当准量度浓;1.745──1N高锰酸钾标溶液1准ml相当氧于亚铜的化克数毫。所得的由氧化铜亚重量按附录,的A表出查相当的还糖原(葡萄糖计以的)量。重还原糖干基含量公式按()3计:算…………………………………………………(3)… h式中:A──由录附A表中查得的还原糖以葡萄(计)糖的量重,m;gW─试样─量,重;gM──样水试百分分,率;%双试结验允许差果小数点及数同1.位.41。注:沸时煮间必须控制在4min内。可先取水05l加碱m酒石性酸铜、甲乙①液各2m5l,节调适好的当火后,力再作样品。②煮沸的后液如溶不呈色蓝,表示量过糖高,减可试少样重,另作量。2还原非测定糖21.铁氰化法钾需仪器和所用同具.1.1。1需所试剂同.112。..211.操方法作分吸取别.11.3.样1品及空白液液5各ml于试中,管先在剧烈沸腾水的浴中加热51im(n样液品非中原糖转还化还为原糖),取迅速出却冷后,加入碱性铁化钾溶液氰5lm,混后匀再,入沸腾水浴中继放续热加2mi0,取出n速冷却后迅,立即1.1按3.3.法方行滴进,分别记定下滴定样液及空品白消液硫代耗硫钠体积(酸)。21..2结果算计还非原含糖量按先式(4公计),算求氧出化品样中总“还原液”所糖0.需N1氰铁钾溶液化需的体所积V4),然(后减去单氧化样独品中液“原还”糖所的需铁化氰钾溶体液(V3)积〔 公式1(〕,最后)再据根4V-3V的结果m()l查表,2即可查得样试含中非原还(以蔗糖糖计)的百分。数……………………………………………………4)(中式:定滴白液空耗消硫代酸硫钠溶液体积ml,;────滴定品液消耗样硫代硫钠酸液体溶积,ml; hV4──化氧品样中总液还原糖需所01.N铁化氰钾溶体积,液lm; hN──硫硫代钠溶酸液当浓度量双试。结验允许果不差过超0.50,求其%平均数,为即测定果。结测结果取小数点后第二位。定21..03.1N氰化钾(铁l)与m非原糖还量对照可查表含。2:注非原还含量以糖糖计算蔗表2。01N.K3Fe(NC6</SU)ml非原还糖% h0.010200.3.0040.05.00.00.670.8000.9010.0.111.0021.30.4011.501.601.70180.190.2.002.10.2202.302.402.502.60.702280..9023003..130.02.303340.3.503.60370.38.0.93040.0.4041.20.3040.05.1000.15.091024.0290..4303.0843.0.80.425.570.060.6270.710.76.8010.86.9100.591001..041.901.1411.9.21132.8133..1813.4134.18.521.75.6111.66.7111.71.6811.58190.1952..00.240 h.404.544.604.700.840490.5005.1.0.2505.30.5405.505.60.570.8055.0960.06.160.26.0306406.5.0.606.706.6086.97.0070.07.2170.3074.0.705.60777.07.80.9708.008.01.280.380.408.850.0292.142.1282.32.282.32.33824.224.72512.5.6261.2662..72.752.0820.082.902.492.93.9043.90.133.3183.3232.83.333.3734.23.437.253.5736.2367.3.7327.7.3283873.92.3.97.0244.07h2 .2林费氏液2法2.1试.剂2.21..16N酸:取盐盐100m酸l加,至水200lm;2..122.基红指示甲液:01.甲基%乙醇溶液红;.2.2132.0%氢氧化溶液;钠22.1..4其余试同1.剂2.。22..22操方作吸取1.法.23.1项已下制备样的品液50lm,注入1000ml容量中瓶,6N盐酸加5m,l在68~07水℃浴加热中15min,冷后却加基甲红指液示2滴,用2%0氢化氧钠液溶中,和加至水刻度混匀,,然按后12.3..2测定样品中液总原糖还。2.2.3果计结算非还糖原基干量(含以蔗糖)计按式(5公)计算:………………………………5)(式中:A──′转化后测得还原糖的(葡萄糖以)计量,重g;Vm─转化─后稀释至100l,m于用测还定原糖体积,ml;的W──测原还定原糖试样时重量,;g h.05─9还─糖(以原萄葡计糖换)算为糖蔗的数因M──;样试水分百率,%。分双验结果允许差及小数点试数同位2..2。1附A录相于当氧亚铜重化量葡萄糖的、糖、果转糖化重量表(充件补)相同于氧亚铜重化量的萄葡糖果糖、、转糖化重量下见:表化亚铜氧葡糖萄果糖mg转化糖 1.312.413.15146.1.51869.1801..910.322142.2523..64.285.292.702.8129330 ..4315.3.2633.834.39.630.23873.39.4405.41.742.83.945.4460.4273.8.4494.55.0751.58295..405.52h46.5.1.5660.6.57.075..808.589..49.99104.0.19114.11.12.93128.13.313.84.311.841.351.756121..7167.2717.1.8281.71.29917.0.212.602.1211.6221.226.23.1236.5.1.566.61.772.7.8.3788.9.39.9104.0.91115.21.012.5131.316.14.124.751.21581.6.3168.1.471.71894.19.01.5920.12.0216.11.72222.22.28.3332.84.242.4925.24.605.257..26677..72.7.28879..2.9710.20.171.211.17213.1.2831.33.8114314.815..35.81163.61.817.31.871.381.8919.4199.2.042.0912.42.192.422.293.52240.2.54520 56..35.475855.9.706.8619.630.64.26.3566.47.668.76698.0.9772.137.74.237.456.6777.78.787.9981.128.23.38844.8568..768.788.980.199.219239.34.496.9.596.8797.9991.h4212..426.125.656.212.527.067.225.028.852.0992.50.030.353103.1.5320.3.5233.0335.4.30345.5.303553.60.3.537.0637.35.8038.539.03.5940.040.51.041454..2042.5430.2.62751.27.628.28.279.229.820.3330.931.431932.53..3303634..13.4735.23.58363.3.86374.7.393.5893.39.604.14007.4.121.744.32428.34.43.4944.545.450.66.4146.47.227.556.206.527.202762..812862..19296.0.13306.132.13.73.2232.73.2333.7343.438.5.333.85363.3.6873.473.938.4389.394.04.040.54.0114.5420.246.431.43.644.144.745.21 0.20101.312.05103.6041.170.8510701.8.10109.2101.31115.121.163.7114.8111.06117.11182.1913.1205.211.6122.723.18125.1026.1127.212.3128.9513061.137.123.814.3013.153612.17.4318351.3.69140.74119.1430h.4.3544.44.505.044.5546.046.5470.74.5840.8.459.049.5405050.65.11.51.62.155.6253.15.365.454.165515.5.66.155.767.255.757.25887.59259.7.60.602.6713.16.86.236.2874.84.8384.994.40.505.5051.1516.52.252.75.3533.84.55449.5.55650.566.57.15.75782.58.85.35999.604.1.06616.62.162.736.263.8463.6.49654.6.0666567.1.7.768.626.88547.4.246.677.4374.84.83488.49.49.945.045095.15.52.52.50530.5.364515..645.25557.56.25.67753.5.8785.35.9859.49.9560.416.061.56.0262.63.1636.64.2664.75.6625.8 14.411452146..414.7514.8641.7190.91552.053.1115.214554.156.5175.615.817599.161016.2.116.21634.1654.5616.667.1168.89107.017.1117.32173.41475.175.617.86177.91790.180.181.1183.24138.51485.18581.8.9h0633.6.836.3644.659.4569.6.6466.96.74680.6.58960.965.70.070.71.517167..1272.63.717.3747.274.75.275.7776.73.68773.7.877.3878.7994.9.978.48110.18.528.028583..1963.9.97604.7.107.6172.1277.372.3.784.737497.5.756.06.6777.177.778.378.87.98040.80.58.181.168.2282883..338.948.458.0856.6.81867.783.788.88.49.8098.90.51906.663.668.6746..9768.46.90965.7007.0.671.171.672272..7 73.73.827.437.497.545.7796577.0.77.6871.78.69.779.28073.808.1.381898.2.4830.83.845084..65818..576.828.86188 018..1919.0311.499125.193.6149.8195.919.0718.9199.31200.421.502027.20.820349.206.0072.228.03290.2140.512.7121.821329.215021.6.2172.238.412195.22.0722.1822.92242.220.52226.3227.224.58292.732.8h08.63481.486.582.8.5786.286.77.387.88883.8.988.4899.90.9491.091592.0.92.693.13.996.42497.9.259.759.369.68973.9799.84.9.98995.100.010.5100.11011.610.22021.71032.01.3819.29.81923.9299..539.0944.65.2995.967.396.997.489098.69..299.9710.301009.11041.200.012.1630.113.70104.3104.81054.16.0010.6610.7110711.0.8318.08109.410.10110.6111.111.71121.3121.9873.8.8887.488.99.859.000.6991.1917.92.29.829.3933.894.449.99.55960.966.9.71977.89.298.8993.99.900.141010.01.5112.1012.6003.211037.10.310448105.410..06106.517.1007.611802 .32.9123.1324.233253.23.6427.3236.872398.20492.421.23.14244.32454.246.6247.728.4824.925911.22.25253.25344255.6.2567.57.8225.98260.2116.226.2323.64246.625.672668.26.8209.6172.207123.2275273.6.74.27h10.43104.8105.41509.106.1057.017.5018.10108.610.9120.9117.0121.0181.3111.9112.4111.9121.5114.3011.411561.11.5711.261617.117.3117.18814.1819.1915.120.02106121.11.12.1272.2122.7132.13238.12.44241.911.3114.041416.11.52115.716.3116.1917.11581011..86191.211.9180.2312.09121.512.212126.13.2212.832414.215.12055.12.1612.761273.17.9218.42291.0129.621.02103.8311313.1.9132.513.133317.134.132.4813.54108.719.030918110..4110.9111.512.11121.116.3213.1114.37114.91154.116.016.111751.17.11168.218.8111.913199.120.141.21210.621.2112.21273.31238.214.4124.9251.156.1212661.7.22127.18283.128.9129.5130. 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h415.542.65534745.4.45680.47.51548.259.3464.5046.616427.6438.64.0566.4147.6462.4869454.0.76741.74279.4470.475.174.6277444.7.547896480..741.8943.0488.4485.1482.64487.458.648897.215.31259.26.5217.112178.28.411290.219.62202.202.822 1.422.0222.622233.223.924.5225.122527.22.36272.02726.22.822288.292.250.13320.731.242230.232.73233.34.0224.73352.33621.32.9632.1023.702313.32.2022.3623.2233.39234.53521.235.8236.234712.3.7237.4829302.397.2403.241024.1.622.2424.2943.26244.324.4245.926463.247.2074.8482.529.2452.0050.822156.522725.3.272.9222352.4.1224272.5242.26.206.262722.27.9222.5829.122297.23.423100.32.12327.3223.293.6234.233428.25.533621.263.823.5738.1232.883925.2402240.8.2415.42.224330.2438244..724.85:摘注自食品卫《生验方法检理化部分2》63242页。~h 加说附明:本准标由中华民共和人商国业提出部。本标准由业商粮部储运局负食起责草。标准本主要草人高起修、杨浩吾然、吴霞、艳吕桂。芬迎您欢的下,资载仅料供考!参