样品化验与质量评述

1、商州区潘河鋁矿区化学样品鋁元素分析质量总结受综合地质大队地调所的委托我室于2010年5月至2011年3月期间承担了商州区潘河 钳矿区化学样品的分析测试工作，分析项口 mo共1种元素o依据dz/t 0130.4-2006及 gb/t14352.2-1993标准要求，我室采用了 721-100分光光度计等仪器进行分析测试。本次工作共采钻孔基本分析样5394件。按照中华人民共和国地质矿产行业标准dz/t 0130.4-2006地质矿产实验室测试质量管理规范第2部分：岩石矿物分析试样制备和第2 部分：岩石矿物样品化学成分分析的要求，分别对样品进行加工和分析测试，具体步骤如f：1、试样制备我室对钳矿石的

2、分析，样品加工遵循切乔特(t e q。t t )经验公式，即：q = kd2 0 样品的k值采用0.5.分析试样的制备分为三个阶段：即粗碎、中碎和细碎。每个阶段又包括 破碎、过筛、混匀和缩分四道工序。分析试样的制备流程见下图过筛(lmm).混勻、缩分细碎弃去粗副样混勻、.缩分分析副样分析止样粗碎阶段损耗率低于3%、中碎阶段低于5%和细碎阶段低于7%, _h.il筛率人于95%。样 品经过加工后，分析样置于6080°c的烘箱屮烘干，分析。2、样品化验选川中华人民共和国国家标准gb/t14352. 1-1993和gb/t14352. 2-1993作为分析钩钳的 主要方法。称0. 1000

3、-0.5000克样品至線堆锅中，经过氧化钠熔融，水浸取，钳呈钳酸盐 进入溶液中，钳酸盐在9% 10%的硫酸介质中以铜盐催化，用硫關将钳还原至五价状态，与 硫議酸盐结合成可溶性橘红色硫氟酸铜络合物，在分光光度计上于波长460nm处测定吸光 度，计算钥量。每一批样品，插入2个或2个以上标准物质或监控样样品平行测定。标准物质插入分 布在该批样品的前、中和后部位。每一批样品随机抽取25%样品作为检查样，并编成密码 交由不同人员分别进行基木分析和检查分析。每一批样品插入2份空白试验，与样品平行测 定，插入位置为前部和肩部。统计棊木分析与内检分析成果的相对偏差，再用dz0130-2006 地质矿产实验室测

4、试质量管理规范中规定的数学模型计算（也可查表求得）相对偏差允许限, 相对偏差小于等于允许限时为合格，大丁允许限时为不合格。在准确度判定后按批次统计试 样的合格率，内检合格率人于95%。皋本分析成果从正样屮抽取样品总数的5%送外检。统计 外检分析成果与基本分析成果的相对偏差，确定相对偏差允许限，在准确度判定后计算合格 率，外检合格率大于90%。达到了dz0130-2006地质矿产实验室测试质量管理规范耍求。3、内、外检质量木次工作共采钻孔基木分析样5394件，内检由陕西省地矿局综合地质大队地调所项目组 抽取粗副样交由我室进行自检代替，自检合格后出具化验报告和对应的口检报告（见附表1）, 共抽取自

5、检样540个,自检率10.01%,大于内检要求的总样品数的10%,内检合格率97.04%, 达到dz0130-2006地质矿产实验室测试质最管理规范要求的内检合格率大于95%.计算公 式如下：相对双差值rd=（基分结果一内验结果）/ （基分结果+内验结果）x100；相对偏差允许限 yc=c （14. 37 t _0 1263-7. 659）yc重复分析试样中mo的相对偏差允许限，t 重复分析试样中mo的平均质量分数，%c-某矿种某组分重复分析相对偏差允许限系数，mo=l当rd> yc时，检验结果为超差。当rd yc时，检验结果为合格。外检样从内验合格口高于矿体边界的副样中提取，至新编号后

6、送西安矿产地质研究所实 验测试中心分析。共抽取外检样270个，占样品总数的5%。外检合格率94. 07%，其中超差16 件，达到wz0130-2006地质矿产实验室测试质量管理规范要求的90%以上。内外检质量统计表见附表2。 附表1内检送样 号原检测结果内检检测结果相对偏差（rd）允许偏潍合格j3 (mo) /10'23 (mo) /10'2(yc)超差x内11.5511.5151.1745.956v内20.0640.076-8.57112.447v内30.1480.152-1.33310.602v内40.1470.164-5.46610.519v内50.0910.097 3.

7、19111.712v内60.1040.112-3.70411.375v内70.0950.098-1.55411.648v内80.1190.1161.27711.174v内90.1010.1125.16411.409v内100.3370.341-0.590&815v内110.0750.0712.74012.340v内120.0950.106-5.47311.549v内130.0790.083-2.46912.080v内140.1070.115-3.60411.309v内150.0480.051-3.03013.346v内160.2010.213 2.8999.874v内170.1480.

8、158-3.26810.556v内180.0840.088-2.32611.931v内190.0480.053-4.95013.293v内200.0780.0833.10612.095v内210.0150.01020.00017.334x内220.0810.086-2.99412.004v内230.0890.092-1.65711.805v内240.0960.103-3.51811.573v内250.0510.057 5.55613.117v内260.1690.1486.62510.475v内270.1630.172-2.68710.349v内280.3090.2981.8129.047v内2

9、90.0340.035-1.44914.326v内300.5640.629-5.4487.680v内310.1100.117-3.08411.256v内320.0610.0582.52112.864v内330.2390.256-3.4349.482v内340.1170.1150.86211.204v内350.0430.044-1.14913.692v内360.0740.0656.47512.465内370.0930.0882.76211.805v内381.2201.0955.4006.448v内390.0670.05212.60512.864v内400.1220.1124.27411.184v

10、内410.0770.080-1.91112.158v内420.0750.0684.89512.393内430.0730.0683.54612.429v内440.1010.0962.53811.598v内450.0790.0659.72212.375v内460.0430.03411.68814.024v内470.0620.0601.63912.799v内480.0660.0595.60012.737v内490.0160.01118.51917.092x内500.2940.2615.9469.237v内510.9080.9381.6256.857v内520.1630.1426.88510.564v

11、内530.1030.08211.35111.751v内540.1120.08911.44311.549v内550.0720.05711.62812.656v内560.0590.04513.46213.216x内570.6260.5873.2157.648vft 580.0760.0657.80112.429v内590.0990.0895.31911.712内600.1200.1047.14311.288v内610.1290.1155.73811.084v内620.1530.1375.51710.680v内630.0730.0628.14812.539v内640.0740.0619.63012.

12、539v内650.1570.1473.28910.571v内660.0890.075&53712.049v内670.0700.05611.11112.716v内680.0440.03314.28614.024x内690.2770.2475.7259.360v内700.1930.1667.52110.192v内710.1090.0956.86311.513v内720.1570.1502.28010.549v内730.0410.0349.33314.096v内740.1250.1106.38311.174v内750.1250.1211.62611.065v内760.0600.04811.1

13、1113.117v内770.0980.0847.69211.791v内780.0990.101-1.00011.561v内790.0740.0693.49712.393内800.0710.0682.15812.465v内810.2870.2801.2359.191v内820.0270.0245.88215.182v内830.2500.2323.7349.540v内840.3180.2835.8249.067v内850.0630.067-3.07712.636v内860.0510.0492.00013.320v内870.3190.2944.0789.026v内880.2360.2193.7369

14、.666v内890.0570.061 3.39012.886v内900.1680.1592.75210.404v内910.0720.085 8.28012.158v内920.0780.084-3.70412.080v内930.0550.063-6.78012.886v内940.1350.1186.71910.999v内950.0800.086-3.61412.019v内960.0780.086-4.87812.049v内970.0780.084-3.70412.080v内980.0870.098-5.94611.751v内990.0700.0653.70412.539v内1000.0360.0

15、371.37014.170v内1010.2120.248-7.8269.642v内1020.0650.079-9.72212.375v内1030.0610.068-5.42612.656v内1040.2350.251-3.2929.522v内1050.5050.574-6.3957.876v内1060.0490.063-12.50013.021v内1070.1230.127-1.60011.027v内1080.1880.209-5.2909.967v内1090.2140.234-4.4649.700v内1100.3070.328-3.3078.952v内1110.0750.088-7.9751

16、2.064v内1120.1140.138-9.52411.008v内1130.1900.209-4.7629.956v内1140.3390.340-0.1478.812v内1150.1170.1201.26611.153v内1160.2670.313-7.9319.143v内1170.2290.245 3.3769.577v内1180.1720.192-5.49510.161v内1190.0860.098-6.52211.765v内1200.1540.181-8.06010.349v内1210.0860.095-4.97211.805v内1220.0650.078-9.09112.393v内1

17、230.0260.032 10.34514.814v内1240.0490.050-1.01013.346v内1250.0670.080-8.84412.323v内1260.0310.0293.33314.718v内1270.0620.072-7.46312.558v内1280.0300.02411.11115.017v内1290.0990.111-5.71411.443v内1300.2840.339-8.828&992v内1310.1280.146-6.56910.812v内1320.0890.108-9.64511.598v内1330.0350.0307.69214.493v内134

18、0.1160.1112.20311.256v内1350.1510.154-0.98410.564v内1360.1200.138 6.97710.953v内1370.1350.151-5.59410.712v内1380.0840.0830.59912.004v内1390.2640.285 3.8259.260v内1400.1380.155-5.80210.656v内1410.0710.0700.70912.429v内1420.0520.055-2.80413.141v内1430.0610.068-5.42612.656v内1440.0610.04910.90913.069v内1450.1040.

19、1040.00011.466v内1460.0700.0644.47812.558v内1470.0960.0893.78411.751v内1480.0820.06313.10312.358x内1490.0780.0733.31112.256v内1500.1240.1058.29711.235v内1510.2310.2231.7629.671v内1520.0550.0477.84313.267v内1530.1460.1267.35310.829v内1540.0480.0409.09113.661v内1550.1200.1133.00411.194v内1560.1860.188-0.53510.10

20、0内1570.1550.182-8.01210.335v内1580.0900.0805.88211.960v内1590.0890.0767.87912.034v内1600.1020.0953.55311.598v内1610.0680.069-0.73012.502内1620.0790.0706.04012.289v内1630.0200.01417.64716.382x内1640.0610.0591.66712.842v内1650.0740.0647.24612.483v内1660.0600.071-8.39712.616v内1670.4490.496-4.9748.138v内1680.0830

21、.0811.22012.049v内1690.0700.0635.26312.577v内1700.0580.0534.50513.045v内1710.2310.2163.3569.705内1720.1980.1697.90210.143v内1730.2640.2522.3269.393v内1740.1070.0984.39011.501v内1750.1020.0915.69911.648v内1760.0300.0267.14314.914v内1770.0670.0596.34912.716v内1780.4380.464-2.8828.231v内1790.1750.1604.47810.349v内

22、1800.2600.271-2.0729.331内1810.0780.0780.00012.174内1820.1600.170-3.03010.383v内1830.1230.1230.00011.065v内1840.0630.0611.61312.757v内1850.0850.092-3.95511.860内1860.1160.1083.57111.288内1870.0920.096-2.12811.712v内1880.2670.272-0.9289.299v内1890.2940.310-2.6499.057v内1900.0960.108 5.88211.513v内1910.1110.117-

23、2.63211.246v内1920.0600.063-2.43912.778v内1930.1020.110-3.77411.420v内1940.1820.216-8.5439.961v内1950.2060.225-4.4089.785v内1960.0800.0790.62912.126v内1970.0980.116-8.41111.398v内1980.1750.209 8.85410.041v内1990.0630.067-3.07712.636v内2000.0670.076-6.29412.393v内2010.0450.047-2.17413.542v内2020.1770.195-4.8391

24、0.112v内2030.2200.239-4.1399.647v内2040.0660.071 3.65012.502v内2050.0660.070-2.94112.521v内2060.0690.083-9.21112.239v内2070.1790.197-4.78710.088v内2080.0830.095-6.74211.846v内2090.4050.452-5.4848.334v内2100.1890.1647.08210.230v内2110.1530.174-6.42210.404v内2120.0480.054 5.88213.267v内2130.0770.097 11.49411.902

25、v内2140.066().08()-9.58912.340v内2150.1440.172-8.86110.482v内2160.2840.31246989.085v内2170.1460.164 5.80610.526v内2180.2590.296-6.6679.237v内2190.0650.072-5.10912.502v内2200.0320.02512.28114.863v内2210.4790.552-7.0817.965v内2221.9561.8263.4375.600v内2230.2080.217 2.1189.816v内2240.3580.371-1.783&665v内2250.

26、0960.0856.07711.805v内2260.1540.179-7.50810.363v内2270.0430.0412.38113.787v内2280.0780.0751.96112.223v内2290.0690.0680.73012.502v内2300.1700.173-0.87510.295v内2310.1930.1900.78310.047v内2320.0660.072-4.34812.483v内2330.0610.0555.17212.930v内2340.0600.0621.63912.799v内2350.1320.145-4.69310.787v内2360.0600.0518.

27、10813.045v内2370.0490.060-10.09213.093v内2380.0830.092-5.14311.888v内2390.1200.133 5.13810.999v内2400.1080.0994.34811.478v内2410.2230.2132.2949.759v内2420.0390.041 2.50013.919v内2430.0770.0695.47912.340v内2440.0630.072 6.66712.539v内2450.0840.0956.14511.832v内2460.1310.143-4.38010.812v内2470.0320.02316.36414.9

28、65x内2480.0820.0763.79712.142v内2490.0670.0623.87612.656v内2500.2170.2052.8449.831v内2510.0330.038-7.04214.247v内2520.5100.4921.7968.022v内2530.0790.0724.63612.256内2540.0880.092-2.22211.819v内2550.1800.1751.40810.218v内2560.0440.0396.02413.819v内2570.0700.0653.70412.539v内2580.0470.0425.61813.631内2590.0600.06

29、8 6.25012.676v内2600.1960.1862.61810.053v内2610.6720.6620.7507.465v内2620.0610.0537.01812.975v内2630.0510.0492.00013.320内2640.0680.05510.56912.778v内2650.0470.03810.58813.755v内2660.0930.078&77211.945v内2670.0800.082-1.23512.080v内2680.1990.231-7.4429.790v内2690.0790.0659.72212.375v内2700.0760.0667.04212.

30、411v内2710.0610.0591.66712.842v内2720.0630.064-0.78712.696v内2730.2400.2311.9119.590v内2740.3410.375-4.749&702v内2750.3530.390-4.980&625v内2760.1930.208-3.7419.945v内2770.3130.365 7.670&815v内2780.0880.093276211.805v内2790.1860.211 6.2979.967v内2800.0790.088-5.38912.004v内2810.0300.034 6.25014.536v

31、内2820.3580.408-6.5278.563v内2830.0650.072-5.10912.502v内2840.0340.02515.25414.765x内2850.1030.104-0.48311.478v内2860.0750.085 6.25012.111v内2870.2020.234-7.3399.759v内2880.7390.813-4.7687.179v内2890.0450.052-7.21613.400v内2900.2110.236-5.5939.705v内2910.0620.073-8.14812.539v内2920.090004-7.21611.635v内2930.273

32、0.282-1.6229.237v内2940.0630.072 6.66712.539v内2950.0650.074-6.47512.465v内2960.2680.296-4.9659.202v内2970.0230.025416715.357v内2980.1920.201-2.2909.989v内2990.1180.120-0.84011.143v内3000.0780.0761.29912.206v内3010.0920.0920.00011.765v内3020.1200.123-1.23511.094v内3030.0340.0331.49314.408v内3040.0840.087-1.754

33、11.945v内3050.1180.1151.2881l194v内3060.1950.201-1.5159.972v内3070.0300.0267.14314.914v内3080.0690.0671.47112.521v内3090.0690.0680.73012.502v内3100.0930.0911.08711.765v内3110.0790.083-2.46912.080v内3120.0800.081-0.62112.095v内3130.0490.054-4.85413.241v内3140.0650.067-1.51512.597v内3150.1170.126-3.70411.094v内31

34、60.0890.095-3.26111.765v内3170.1380.1360.73010.812v内3180.1260.129 1.17610.980v内3190.1010.106-2.41511.478v内3200.0540.057-2.70313.045v内3210.0620.0620.00012.757v内3220.0330.034-1.49314.408v内3230.1030.1020.48811.501v内3240.1290.1155.73811.084v内3250.1580.164-1.86310.439内3260.1470.159-3.92210.556内3270.1180.1

35、122.60911.225v内3280.1020.1000.99011.537v内3290.0380.0371.33314.096v内3300.0640.068-3.03012.597内3310.0970.0837/77811.819v内3320.0560.0532.75213.093v内3330.0880.0757.97512.064v内3340.1790.1780.28010.205v内3350.1330.1128.57111.075v内3360.3880.391 0.385&528v内3370.0320.02316.36414.965x内3380.0840.0709.09112.

36、206内3390.0800.0800.00012.111v内3400.1030104-0.48311.478内3410.1020.1010.49311.525内3420.0150.0150.00016.765v内3430.1000.103-1.47811.525v内3440.0890.0833.48811.931v内3450.0390.0372.63214.060v内3460.0810.0781.88712.126v内3470.0420.0376.32913.954v内3480.0610.0600.82612.821v内3490.0930.0798.14011.931v内3500.0450.0

37、3315.38513.988x内3510.2350.244-1.8799.554v内3520.1140.1130.44111.256v内3530.1000.0933.62711.648v内3540.1760.1701.73410.276v内3550.0470.0443.29713.571v内3560.2160.224-1.8189.739v内3570.0900.0862.27311.874v内3580.0520.0510.97113.241v内3590.0350.0299.37514.536v内3600.0870.0851.16311.931v内3610.0720.081-5.88212.22

38、3v内3620.0430.048-5.49513.571v内3630.0680.074-4.22512.411v内3640.0740.083-5.73212.158v内3650.0900.108-9.09111.586v内3660.0600.075-11.11112.539v内3670.1850.195 2.63210.065v内3680.1540.164-3.14510.468v内3690.2770.295-3.1479.172v内3700.0310.02216.98115.071x内3710.1290.150-7.52710.770v内3720.0670.076-6.29412.393v内

39、3730.1270.136-3.42210.908v内3740.0620.070-6.06112.597v内3750.0380.03011.76514.367v内3760.0720.077-3.35612.289v内3770.0920.0901.09911.791v内3780.0660.0641.53812.636v内3790.3410.378-5.146&693v内3800.0780.085-4.29412.064v内3810.0600.0621.63912.799v内3820.0760.081-3.18512.158v内3830.0360.0360.00014.208v内3840.

40、0350.02712.90314.625v内3850.1170.121-1.68111.143v内3860.1380.1360.73010.812内3870.1320.1300.76310.917v内3880.0380.0345.55614.208v内3890.0950.0931.06411.712v内3900.1480.1451.02410.656v内3910.0300.0291.69514.765内3920.1980.1785.31910.088v内3930.1380.155-5.80210.656v内3940.0640.065-0.77512.656v内3950.2290.248-3.9

41、839.563v内3960.1990.215-3.8659.874v内3970.0450.046-1.09913.571v内3980.3780.389-1.4348.560v内3990.0700.078-5.40512.306v内4000.0690.0662.22212.539v内4010.2240.260-7.4389.531v内4020.0640.073 6.56912.502v内4030.0750.089-8.53712.049v内4040.1600.180 5.88210.315v内4050.0410.045-4.65113.723v内4060.1190.142-8.81210.926

42、v内4070.0780.088-6.02412.019v内4080.0610.070-6.87012.616v内4090.0720.091 11.65612.064v内4100.0620.063-0.80012.737v内4110.0480.0480.00013.428v内4120.1350.152-5.92310.704v内4130.0690.075-4.16712.375v内4140.0460.0406.97713.723v内4152.0381.8754.1665.543v内4160.1270.148-7.63610.803v内4170.0600.061 0.82612.821v内4180.3000.335-5.512&952v内4190.0640.073-6.56912.502v内4200.1020.120&10811.309v内4210.0140.020-17.64716.382x内4220.0510.056-4.67313.141v内4230.0990.112-6.1